CN111968821A - Soft magnetic alloy powder and preparation method thereof, and magnetic ring inductor and preparation method thereof - Google Patents
Soft magnetic alloy powder and preparation method thereof, and magnetic ring inductor and preparation method thereof Download PDFInfo
- Publication number
- CN111968821A CN111968821A CN202010720769.6A CN202010720769A CN111968821A CN 111968821 A CN111968821 A CN 111968821A CN 202010720769 A CN202010720769 A CN 202010720769A CN 111968821 A CN111968821 A CN 111968821A
- Authority
- CN
- China
- Prior art keywords
- powder
- alloy
- amorphous
- alloy powder
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 295
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 50
- 229910001004 magnetic alloy Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000000956 alloy Substances 0.000 claims abstract description 113
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 110
- 238000000034 method Methods 0.000 claims abstract description 62
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 57
- 239000010959 steel Substances 0.000 claims abstract description 57
- 238000000889 atomisation Methods 0.000 claims abstract description 51
- 238000002425 crystallisation Methods 0.000 claims abstract description 41
- 230000008025 crystallization Effects 0.000 claims abstract description 41
- 239000010949 copper Substances 0.000 claims abstract description 35
- 238000000137 annealing Methods 0.000 claims abstract description 34
- 229910052802 copper Inorganic materials 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 239000002245 particle Substances 0.000 claims abstract description 27
- 230000008569 process Effects 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000001301 oxygen Substances 0.000 claims abstract description 22
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 22
- 229910052742 iron Inorganic materials 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 19
- 238000009826 distribution Methods 0.000 claims abstract description 18
- 238000009689 gas atomisation Methods 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 238000001291 vacuum drying Methods 0.000 claims abstract description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910000592 Ferroniobium Inorganic materials 0.000 claims abstract description 15
- ZFGFKQDDQUAJQP-UHFFFAOYSA-N iron niobium Chemical compound [Fe].[Fe].[Nb] ZFGFKQDDQUAJQP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims abstract description 15
- 238000012216 screening Methods 0.000 claims abstract description 15
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 14
- 239000010431 corundum Substances 0.000 claims abstract description 14
- 238000003723 Smelting Methods 0.000 claims description 63
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 229910052796 boron Inorganic materials 0.000 claims description 14
- 229910052758 niobium Inorganic materials 0.000 claims description 14
- 230000001681 protective effect Effects 0.000 claims description 14
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- 239000004571 lime Substances 0.000 claims description 13
- 229910052698 phosphorus Inorganic materials 0.000 claims description 13
- 238000012545 processing Methods 0.000 claims description 13
- 238000003825 pressing Methods 0.000 claims description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 230000002829 reductive effect Effects 0.000 claims description 4
- 229920002050 silicone resin Polymers 0.000 claims description 4
- OSMSIOKMMFKNIL-UHFFFAOYSA-N calcium;silicon Chemical compound [Ca]=[Si] OSMSIOKMMFKNIL-UHFFFAOYSA-N 0.000 claims description 3
- 239000002893 slag Substances 0.000 claims description 3
- 230000006698 induction Effects 0.000 abstract description 16
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 238000002844 melting Methods 0.000 abstract description 3
- 230000008018 melting Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 17
- 229910052918 calcium silicate Inorganic materials 0.000 description 10
- 239000000378 calcium silicate Substances 0.000 description 10
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- 239000002131 composite material Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910000859 α-Fe Inorganic materials 0.000 description 4
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 229910001111 Fine metal Inorganic materials 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000006247 magnetic powder Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000007578 melt-quenching technique Methods 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002707 nanocrystalline material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000009692 water atomization Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15308—Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
-
- 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
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15333—Amorphous metallic alloys, e.g. glassy metals containing nanocrystallites, e.g. obtained by annealing
-
- 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
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15341—Preparation processes therefor
- H01F1/1535—Preparation processes therefor by powder metallurgy, e.g. spark erosion
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F17/00—Fixed inductances of the signal type
- H01F17/04—Fixed inductances of the signal type with magnetic core
- H01F17/06—Fixed inductances of the signal type with magnetic core with core substantially closed in itself, e.g. toroid
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/24—Magnetic cores
- H01F27/255—Magnetic cores made from particles
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Dispersion Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses soft magnetic alloy powder and a preparation method thereof, a magnetic ring inductor and a preparation method thereof, belongs to the field of alloy materials, and is characterized in that industrial pure iron with the purity of 99.9 percent, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus are selected as raw materials, a corundum crucible is added for steel burning, a supersonic speed gas atomization nozzle is adopted, and the powder obtained by atomization is subjected to water-powder separation and vacuum drying to obtain a required amorphous powder precursor; and the required amorphous nano magnetically soft alloy powder is obtained through the combined batch treatment of crystallization annealing treatment, powder grading and screening. The invention has the beneficial effects that: through medium-frequency induction melting, gas-jet water-cooling atomization, and the matching of later-stage water-powder separation, vacuum drying, crystallization annealing treatment, powder grading, screening and other processes, the prepared powder has the characteristics of good sphericity, low oxygen content, reasonable particle size distribution and the like.
Description
Technical Field
The invention relates to the field of alloy materials, in particular to soft magnetic alloy powder and a preparation method thereof, and a magnetic ring inductor and a preparation method thereof.
Background
With the increasing requirements of the electronic market for high frequency, light weight, miniaturization and high performance of components, amorphous nanocrystalline two-phase composite soft magnetic alloy materials with fine and uniform crystalline phases (usually less than 50nm) are receiving increasing attention. The alloy can be obtained by crystallization heat treatment of amorphous material, namely, an amorphous precursor is prepared by a melt quenching method, and then the alloy is obtained by crystallization annealing treatment at proper temperature. The typical microstructure of the Fe-based nanocrystalline soft magnetic material is composed of an amorphous phase matrix and alpha-Fe (Si) nanocrystalline phase phases dispersed and distributed on the amorphous phase matrix. The fine nanocrystalline grains are uniformly distributed on the amorphous matrix, so that the alloy shows better comprehensive performance with polycrystalline materials or amorphous materials, such as higher strength, specific heat, saturated magnetic induction intensity, magnetic conductivity, good plastic deformation capability and stability, lower coercive force and loss and the like.
For the soft magnetic composite material, when the basic component, namely the alloy component of the powder, is selected, the magnetic permeability and the loss of the soft magnetic composite material are mainly related to the appearance, the particle size, the coating process and the heat treatment condition of the magnetic powder. The most of the existing amorphous nanocrystalline magnetic powder core powder is from the breakage of strip-shaped amorphous materials, and the soft magnetic performance of the powder is sharply deteriorated due to the fact that the insulating layer is easily punctured in the pressing process of the powder core due to the sharp edge of the powder.
For example, chinese patent CN104934179B discloses an iron-based nanocrystalline magnetically soft alloy with strong amorphous forming ability and a preparation method thereof, wherein the expression of the alloy is FexSiaBbPcNbdCue, and x, a, b, c, d and e in the expression respectively represent the atomic percentage content of each corresponding component, and satisfy the following conditions: a is more than or equal to 0.5 and less than or equal to 12, b is more than or equal to 0.5 and less than or equal to 5, c is more than or equal to 0.5 and less than or equal to 12, d is more than or equal to 0.1 and less than or equal to 3, x is more than or equal to 70 and less than or equal to 85, and x + a + b + c + d + e is 100 percent.
Disclosure of Invention
Aiming at the problem that the soft magnetic performance of the soft magnetic composite material in the prior art is rapidly deteriorated due to the fact that an insulating layer is easy to pierce in the powder core pressing process, the amorphous nanocrystalline FeCuNbSiBP alloy powder prepared by preparing an amorphous powder precursor with an alloy component in a mode of air-jet water-cooling atomization and carrying out crystallization annealing treatment on the amorphous powder precursor by combining with a corresponding heat treatment process has the advantages of being good in sphericity, high in tap density, good in powder dispersibility, low in powder oxygen content and the like, and provides industrial demonstration for large-scale production of iron-based amorphous nanocrystalline magnetic ring inductors. The specific technical scheme is as follows:
a preparation method of amorphous nano soft magnetic alloy powder comprises the following components in percentage by mass: 6-9% of Si, 1-2.5% of B, 1-3% of Cu, 4-7% of Nb, 0.5-2% of P and 82-87.5% of Fe.
Preferably, the components of the obtained alloy powder are respectively as follows by mass percent: 6.5% Si, 1.7% B, 1.5% Cu, 5.8% Nb, 0.5% P, and the balance Fe.
Preferably, the method comprises the following steps:
the method comprises the following steps: alloy smelting, namely proportioning according to alloy components, selecting industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus with the purity of 99.9 percent as raw materials, adding the alloy raw materials into a corundum crucible for steel burning, and smelting by adopting medium-frequency induction;
step two: performing gas-jet water-cooling atomization to prepare powder, and performing water-powder separation and vacuum drying on powder obtained by atomization by adopting a supersonic gas atomization nozzle to obtain a required amorphous powder precursor;
step three: performing crystallization annealing treatment, namely performing crystallization annealing treatment on atomized amorphous powder at 500-600 ℃ for 60-90min by using high-purity hydrogen with the dew point of-60 ℃ as protective atmosphere to obtain amorphous/nanocrystalline magnetically soft alloy powder;
step four: powder grading and screening, wherein the powder granularity and distribution are controlled by air classification, and the powder laser granularity D50 is controlled: 13-17 μm.
Step five: and carrying out batch processing to obtain the required amorphous nano soft magnetic alloy powder.
Preferably, the ring-hole type supersonic gas atomizing nozzle is adopted in the second step, the inner diameter of the leakage pipe of the tundish is 5.0-6.0mm, and the atomizing pressure is 6-8 MPa.
Preferably, the ring hole type supersonic gas atomizing nozzle is HK-03.
Preferably, in the step one, the smelting power is controlled to be 200-80.0 KW, the smelting time is 60.0-80.0 minutes, when the temperature of the molten steel reaches 1500-1520 ℃, the power is reduced to be 100-150KW, a proper amount of calcium silicon and lime are adopted to carry out slagging and deoxidation treatment on the molten steel, the process time is 10.0-15.0 minutes, and then the molten steel is subjected to slag skimming and steel casting.
Preferably, the powder laser particle size D50 in step four: 13-17 μm, oxygen content of powder is less than or equal to 0.1 wt%, and tap density of powder is more than or equal to 4.5g/cm 3.
The invention also provides amorphous nano soft magnetic alloy powder prepared by the preparation method.
The invention also provides a preparation method of the magnetic ring inductor, which comprises the following steps:
the method comprises the following steps: coating the amorphous nano magnetically soft alloy powder with 1 wt% of KH-550 silane coupling agent and 2 wt% of DC-805 silicone resin, granulating on a granulator to obtain particles with the fineness of 40 meshes, and baking for 1h at 100 ℃;
step two: and (3) taking 27g of the granulation powder obtained after drying in the step one, maintaining the pressure for 3s under the pressure of 1200MPa, and performing cold pressing to obtain the required magnetic ring inductor.
The invention also provides a magnetic ring inductor which is prepared by the preparation method and has the specification of the outer diameter phi 27mm multiplied by the inner diameter phi 14.5 mm; f is 100kHz, under the condition of 1V, the inductance value Ls of the magnetic ring is more than or equal to 60 mu H, the magnetic conductivity mu is more than or equal to 50, the loss Ps is less than or equal to 500kW/m3。
The amorphous nanocrystalline alloy mainly contains ferromagnetic elements such as Fe, Co, Ni and the like; metalloid elements such as Si, B, P, etc. having an effect of improving amorphous forming ability and thermal stability, and noble metal elements such as Cu, Ag, etc. at sites where nanocrystal nuclei are provided, and non-magnetic transition metal elements such as Nb, Zr, V, etc. improving amorphous forming ability and hindering nanocrystal growth. The types and contents of various alloy elements have great influence on the amorphous forming capability, the crystallization process, the microstructure and the magnetic performance of the final nanocrystalline alloy.
Si and B are elements for improving the amorphous forming ability and the thermal stability of the alloy. The alloy has great atomic size difference with Fe element, so that the alloy stack is more compact, and the nucleation is inhibited to be beneficial to amorphous formation. Si is an important non-crystallizing element, the saturation magnetic induction intensity of the alloy is reduced when the content is too high, and the alloy is not easy to form non-crystal when the content is too low. In addition, Si is also a basic constituent element of the nanocrystalline phase α -Fe (Si) phase. The B element is characterized by smaller atomic radius, less outer layer electrons, is very beneficial to the formation of amorphous alloy and is a constituent element of almost all nanocrystalline soft magnetic alloys. In addition, the addition of P reduces the melting point of the alloy and also has the function of improving the thermal stability of the amorphous alloy.
According to the structural requirement of the nanocrystalline alloy, a small amount of Cu and Nb elements are added on the basis of the FeSiBP alloy to obtain the FeCuNbSiBP alloy. The solid solubility of Cu element in Fe matrix is very small, the matrix is easy to separate out in the initial crystallization stage to form a phase-rich area of Cu element, a nucleation position is provided in the crystallization process of the nanocrystalline alloy, and then the further growth of crystal grains is hindered around the alpha-Fe (Si) phase to reduce the size of nanocrystalline crystal grains. Nb is also a key element formed by the iron-based nanocrystalline alloy, the addition of Nb not only improves the iron-based amorphous forming capability, but also has larger atomic radius of Nb, is slowly diffused, and other elements form a structure for inhibiting the precipitation of a primary crystal phase in the nanocrystalline forming process and also prevent alpha-Fe (Si) phase grains from growing.
The air-jet water-cooling atomization powder preparation mechanism is that in an atmospheric environment, molten steel is poured into a heat-insulating tundish through an intermediate frequency furnace and flows into an atomization area through a leakage hole at the bottom of the tundish, the molten steel is impacted by supersonic airflow passing through a nozzle in the process, atomized and crushed into a large number of fine metal droplets, and the droplets form spheres under the action of surface tension in the flying sedimentation process and finally fall into a powder collecting tank to be cooled and solidified into spherical powder particles.
Amorphous powderFinal crystallization annealing treatment: bringing the amorphous powder to a predetermined temperature (which is higher than the initial crystallization temperature T) at a heating rateX1And lower than the second crystallization temperature TX2And is slightly higher than TX1) And preserving the temperature for a period of time at the temperature, finishing the conversion of the powder from an amorphous state to an amorphous/nanocrystalline composite two-phase structure, and then cooling in a furnace or in an air manner to obtain FeCuNbSiBP amorphous/nanocrystalline powder.
The amorphous nanocrystalline soft magnetic alloy powder for the magnetic ring inductor has the important parameters of the used powder such as particle size, morphology, chemical composition, phase structure and the like. The particle size distribution is reasonable, the sphericity is good, the surface is smooth and clean, and the pressing density of the prepared magnetic ring inductor is high; and the atomized amorphous powder is subjected to crystallization annealing to obtain an amorphous and nanocrystalline two-phase organization structure with good soft magnetic performance, and the prepared inductor has excellent comprehensive soft magnetic performance such as excellent direct current superposition characteristic, high frequency, low loss, strong breakdown resistance, high magnetic permeability and the like.
The technical scheme of the invention has the following beneficial effects:
(1) through medium-frequency induction melting, gas-jet water-cooling atomization, and the matching of later-stage water-powder separation, vacuum drying, crystallization annealing treatment, powder grading, screening and other processes, the prepared powder has the characteristics of good sphericity, low oxygen content, reasonable particle size distribution and the like.
(2) The method is characterized in that the performance requirements of sphericity, tap density, powder dispersibility and the like are comprehensively considered, the matching proportion of the raw materials of industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus is reasonably set, an air-jet water-cooling atomization process is adopted after smelting, molten steel is impacted by supersonic airflow through a nozzle, atomized and crushed into a large number of fine metal droplets, the droplets form spheres under the action of surface tension in the flying sedimentation process, and finally fall into powder collection tank water to be cooled and solidified into spherical powder particles; through the design of a nozzle structure, the inner diameter of a tundish leakage pipe and the atomization pressure in the gas-jet water-cooling atomization process, molten steel can be rapidly and uniformly atomized and crushed in the supersonic airflow impact process, and powder formed by falling into a powder collection tank through cooling has good sphericity, low oxygen content and reasonable particle size distribution. Through testing, the powder laser particlesDegree D50: 13-17 μm, oxygen content of powder is less than or equal to 0.1 wt%, and tap density of powder is more than or equal to 4.5g/cm3。
(3) KH-550 silane coupling agent and DC-805 silicon resin are adopted to coat amorphous nanocrystalline soft magnetic alloy powder for granulation, then the powder is pressed into an annular magnetic ring inductor, and the pressing process is controlled to maintain the pressure for 3s under the pressure of 1200MPa, so that the magnetic ring inductor is obtained. The inductance Ls of the magnetic ring inductor is tested by a TH2816B/TH2826LCR tester under the conditions that f is 100kHz and 1V, and the loss value of the magnetic ring inductor is tested by an MATS-2010SA soft magnetic alloy alternating current measuring device under the conditions that Bm is 100T and f is 100 kHz. The inductance Ls of the magnetic ring inductor is more than or equal to 60 muH, the magnetic conductivity mue is more than or equal to 50, and the loss Ps is less than or equal to 500kW/m3。
(4) The FeCuNbSiBP amorphous nanocrystalline magnetically soft alloy powder is prepared by adopting a gas-jet water-cooling atomization powder preparation process, so that the prepared magnetically soft alloy powder has good sphericity, high tap density, good powder dispersibility and low powder oxygen content, and the prepared magnetic ring inductor has the characteristics of excellent direct-current superposition characteristic, high frequency, low loss, strong breakdown resistance and high magnetic conductivity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is an XRD diffraction pattern of a prepared metal powder in accordance with a first embodiment of the present invention;
FIG. 2 is an SEM image of a metal powder prepared according to a first embodiment of the invention;
FIG. 3 is an SEM image of metal powder prepared in comparative example one of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The method adopts an air-jet water-cooling atomization mode to prepare the amorphous powder precursor containing the alloy components FeCuNbSiBP, and combines a corresponding heat treatment process to carry out crystallization annealing treatment on the amorphous alloy precursor to prepare the amorphous nanocrystalline FeCuNbSiBP alloy powder, which has the characteristics of good sphericity, high tap density, good powder dispersibility, low powder oxygen content and the like.
A preparation method of amorphous nano soft magnetic alloy powder comprises the following components in percentage by mass: 6-9% of Si, 1-2.5% of B, 1-3% of Cu, 4-7% of Nb, 0.5-2% of P and 82-87.5% of Fe. The method comprises the following specific steps:
the method comprises the following steps: alloy smelting, wherein the alloy components are proportioned, industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus with the purity of 99.9 percent are selected as raw materials, the alloy raw materials are added into a corundum crucible, the smelting power is controlled to be 200 plus materials and 300KW, the smelting time is 60.0-80.0 minutes, when the temperature of molten steel reaches 1500 plus materials and 1520 ℃, the power is reduced to 100 plus materials and 150KW, a proper amount of calcium silicon and lime are adopted to carry out slagging and deoxidation treatment on the molten steel, the process time is 10.0-15.0 minutes, then, the slag is removed completely, and steel is poured. Wherein the smelting adopts medium frequency induction smelting.
Step two: performing gas-jet water-cooling atomization to prepare powder, namely preparing powder by adopting an HK-03 annular hole type supersonic gas atomization nozzle, wherein the inner diameter of a leakage pipe of a tundish is 5.0-6.0mm, the atomization pressure is 6-8MPa, and performing water-powder separation and vacuum drying on powder obtained by atomization to obtain a required amorphous powder precursor;
step three: performing crystallization annealing treatment, namely performing crystallization annealing treatment on atomized amorphous powder at 500-600 ℃ for 60-90min by using high-purity hydrogen with the dew point of-60 ℃ as protective atmosphere to obtain amorphous/nanocrystalline magnetically soft alloy powder;
step four: powder grading and screening, wherein the powder granularity and distribution are controlled by air classification, and the powder laser granularity D50 is controlled: 13-17 μm. Powder laser particle size D50: 13-17 μm, oxygen content of powder is less than or equal to 0.1 wt%, and tap density of powder is more than or equal to 4.5g/cm3。
Step five: and carrying out batch processing to obtain the required amorphous nano soft magnetic alloy powder.
As a preferred embodiment, the alloy powder obtained by the method comprises the following components in percentage by mass: 6.5% Si, 1.7% B, 1.5% Cu, 5.8% Nb, 0.5% P, and the balance Fe.
The embodiment also provides amorphous nano soft magnetic alloy powder prepared by the preparation method.
The embodiment also provides a preparation method of the magnetic ring inductor, which is characterized by comprising the following steps:
the method comprises the following steps: coating the amorphous nano magnetically soft alloy powder with 1 wt% of KH-550 silane coupling agent and 2 wt% of DC-805 silicone resin, granulating on a granulator to obtain particles with the fineness of 40 meshes, and baking for 1h at 100 ℃;
step two: and (3) taking 27g of the granulation powder obtained after drying in the step one, maintaining the pressure for 3s under the pressure of 1200MPa, and performing cold pressing to obtain the required magnetic ring inductor.
The embodiment also provides a magnetic ring inductor which is prepared by the preparation method and has the specification of 27mm of outer diameter and 14.5mm of inner diameter; f is 100kHz, under the condition of 1V, the inductance value Ls of the magnetic ring is more than or equal to 60 mu H, the magnetic conductivity mu is more than or equal to 50, the loss Ps is less than or equal to 500kW/m3。
The beneficial effects of the powder and the annular inductor obtained by the technical solution of the present embodiment are further described below by several sets of examples and comparative examples.
The first embodiment is as follows:
the preparation method of the amorphous nano soft magnetic alloy powder in the embodiment comprises the following specific steps:
the method comprises the following steps: alloy smelting, wherein the alloy powder comprises the following components in percentage by mass: 6.5% Si, 1.7% B, 1.5% Cu, 5.8% Nb, 0.5% P, and the balance Fe. The method comprises the steps of proportioning according to alloy components, selecting industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus with the purity of 99.9 percent as raw materials, adding the alloy raw materials into a corundum crucible, controlling the smelting power to be 250KW, smelting for 70 minutes, carrying out slagging and deoxidation treatment on molten steel by adopting a proper amount of calcium silicate and lime when the temperature of the molten steel reaches 1500 ℃, reducing the power to be 120KW, and carrying out slagging-off and deoxidation treatment on the molten steel for 10 minutes, then completely slagging off, and pouring steel. Wherein the smelting adopts medium frequency induction smelting.
Step two: performing gas-jet water-cooling atomization to prepare powder, namely preparing powder by adopting an HK-03 annular hole type supersonic gas atomization nozzle, wherein the inner diameter of a leakage pipe of a tundish is 5.5mm, the atomization pressure is 6MPa, and performing water-powder separation and vacuum drying on powder obtained by atomization to obtain a required amorphous powder precursor;
step three: performing crystallization annealing treatment, namely performing crystallization annealing treatment on the atomized amorphous powder at 500 ℃ for 60min by using high-purity hydrogen with the dew point of-60 ℃ as protective atmosphere to obtain amorphous/nanocrystalline magnetically soft alloy powder;
step four: powder grading and screening, wherein the powder granularity and distribution are controlled by air classification, and the powder laser granularity D50 is controlled: 13-17 μm. Powder laser particle size D50: 13-17 μm, oxygen content of powder is less than or equal to 0.1 wt%, and tap density of powder is more than or equal to 4.5g/cm3。
Step five: and carrying out batch processing to obtain the required amorphous nano soft magnetic alloy powder.
Example two:
the preparation method of the amorphous nano soft magnetic alloy powder in the embodiment comprises the following specific steps:
the method comprises the following steps: alloy smelting, wherein the alloy powder comprises the following components in percentage by mass: 7% of Si, 2.1% of B, 1.5% of Cu, 5.8% of Nb, 0.2% of P and the balance of Fe. The method comprises the steps of proportioning according to alloy components, selecting industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus with the purity of 99.9 percent as raw materials, adding the alloy raw materials into a corundum crucible, controlling the smelting power to be 200KW, smelting for 60 minutes, carrying out slagging and deoxidation treatment on molten steel by adopting a proper amount of calcium silicate and lime when the temperature of the molten steel reaches 1520 ℃ and the reduction power is 100KW, and carrying out slagging-off and deoxidation treatment on the molten steel for 15 minutes, then completely slagging off, and pouring steel. Wherein the smelting adopts medium frequency induction smelting.
Step two: performing gas-jet water-cooling atomization to prepare powder, namely preparing powder by adopting an HK-03 annular hole type supersonic gas atomization nozzle, wherein the inner diameter of a leakage pipe of a tundish is 5.5mm, the atomization pressure is 6MPa, and performing water-powder separation and vacuum drying on powder obtained by atomization to obtain a required amorphous powder precursor;
step three: performing crystallization annealing treatment, namely performing crystallization annealing treatment on the atomized amorphous powder at 500 ℃ for 60min by using high-purity hydrogen with the dew point of-60 ℃ as protective atmosphere to obtain amorphous/nanocrystalline magnetically soft alloy powder;
step four: powder grading and screening, wherein the powder granularity and distribution are controlled by air classification, and the powder laser granularity D50 is controlled: 13-17 μm. Powder laser particle size D50: 13-17 μm, oxygen content of powder is less than or equal to 0.1 wt%, and tap density of powder is more than or equal to 4.5g/cm3。
Step five: and carrying out batch processing to obtain the required amorphous nano soft magnetic alloy powder.
Example three:
the preparation method of the amorphous nano soft magnetic alloy powder in the embodiment comprises the following specific steps:
the method comprises the following steps: alloy smelting, wherein the alloy powder comprises the following components in percentage by mass: 6.5% Si, 1.7% B, 1.5% Cu, 5.8% Nb, 0.5% P, and the balance Fe. The method comprises the steps of proportioning according to alloy components, selecting industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus with the purity of 99.9 percent as raw materials, adding the alloy raw materials into a corundum crucible, controlling the smelting power to be 230KW, smelting the raw materials for 80 minutes, reducing the power to be 150KW when the temperature of molten steel reaches 1510 ℃, carrying out slagging and deoxidizing treatment on the molten steel by adopting a proper amount of calcium silicate and lime, wherein the process time is 12 minutes, then completely slagging off, and pouring steel. Wherein the smelting adopts medium frequency induction smelting.
Step two: performing gas-jet water-cooling atomization to prepare powder, namely preparing powder by adopting an HK-03 annular hole type supersonic gas atomization nozzle, wherein the inner diameter of a leakage pipe of a tundish is 5.5mm, the atomization pressure is 8MPa, and performing water-powder separation and vacuum drying on powder obtained by atomization to obtain a required amorphous powder precursor;
step three: performing crystallization annealing treatment, namely performing crystallization annealing treatment on the atomized amorphous powder at 500 ℃ for 60min by using high-purity hydrogen with the dew point of-60 ℃ as protective atmosphere to obtain amorphous/nanocrystalline magnetically soft alloy powder;
step four: powder grading and screening, wherein the powder granularity and distribution are controlled by air classification, and the powder laser granularity D50 is controlled: 13-17 μm. Powder laser particle size D50: 13-17 μm, oxygen content of powder is less than or equal to 0.1 wt%, and tap density of powder is more than or equal to 4.5g/cm3。
Step five: and carrying out batch processing to obtain the required amorphous nano soft magnetic alloy powder.
Example four:
the preparation method of the amorphous nano soft magnetic alloy powder in the embodiment comprises the following specific steps:
the method comprises the following steps: alloy smelting, wherein the alloy powder comprises the following components in percentage by mass: 6.5% Si, 1.7% B, 1.5% Cu, 5.8% Nb, 0.5% P, and the balance Fe. The method comprises the steps of proportioning according to alloy components, selecting industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus with the purity of 99.9 percent as raw materials, adding the alloy raw materials into a corundum crucible, controlling the smelting power to be 300KW, smelting for 60 minutes, carrying out slagging and deoxidation treatment on molten steel by adopting a proper amount of calcium silicate and lime when the temperature of the molten steel reaches 1520 ℃ and the reduction power is 110KW, and carrying out slagging-off and deoxidation treatment on the molten steel for 12 minutes, then completely slagging off, and pouring steel. Wherein the smelting adopts medium frequency induction smelting.
Step two: performing gas-jet water-cooling atomization to prepare powder, namely preparing powder by adopting an HK-03 annular hole type supersonic gas atomization nozzle, wherein the inner diameter of a leakage pipe of a tundish is 5.5mm, the atomization pressure is 6MPa, and performing water-powder separation and vacuum drying on powder obtained by atomization to obtain a required amorphous powder precursor;
step three: performing crystallization annealing treatment, namely performing crystallization annealing treatment on the atomized amorphous powder at 560 ℃ for 80min by using high-purity hydrogen with the dew point of-60 ℃ as protective atmosphere to obtain amorphous/nanocrystalline magnetically soft alloy powder;
step four: powder grading and screening, wherein the powder granularity and distribution are controlled by air classification, and the powder laser granularity D50 is controlled: 13-17 μm. Powder laser particle size D50: 13-17 μm, oxygen content of powder is less than or equal to 0.1 wt%, and tap density of powder is more than or equal to 4.5g/cm3。
Step five: and carrying out batch processing to obtain the required amorphous nano soft magnetic alloy powder.
Comparative example one:
the preparation method of the amorphous nano magnetically soft alloy powder in the comparative example comprises the following specific steps:
the method comprises the following steps: alloy smelting, wherein the alloy powder comprises the following components in percentage by mass: 6.5% Si, 1.7% B, 1.5% Cu, 5.8% Nb, 0.5% P, and the balance Fe. The method comprises the steps of proportioning according to alloy components, selecting industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus with the purity of 99.9 percent as raw materials, adding the alloy raw materials into a corundum crucible, controlling the smelting power to be 250KW, smelting for 70 minutes, carrying out slagging and deoxidation treatment on molten steel by adopting a proper amount of calcium silicate and lime when the temperature of the molten steel reaches 1500 ℃, reducing the power to be 120KW, and carrying out slagging-off and deoxidation treatment on the molten steel for 10 minutes, then completely slagging off, and pouring steel. Wherein the smelting adopts medium frequency induction smelting.
Step two: the water-gas combined water atomization powder preparation adopts nitrogen as process protective atmosphere, and the nitrogen flow is 25.0m3H; in the atomization process, a 35 DEG/25 DEG main and auxiliary spray disk and a double V-shaped nozzle are adopted, the size of a leakage hole at the bottom of a molten steel tundish is 5.0mm, the atomization pressure is 100MPa, and the atomization water flow is 120L/min; carrying out water-powder separation and vacuum drying on the powder obtained by atomization to obtain a required amorphous powder precursor;
step three: performing crystallization annealing treatment, namely performing crystallization annealing treatment on the atomized amorphous powder at 500 ℃ for 60min by using high-purity hydrogen with the dew point of-60 ℃ as protective atmosphere to obtain amorphous/nanocrystalline magnetically soft alloy powder;
step four: powder grading and screening, wherein the powder granularity and distribution are controlled by air classification, and the powder laser granularity D50 is controlled: 13-17 μm. Powder laser particle size D50: 13-17 μm, powder oxygen content less than or equal to 0.1 wt%The powder tap density is more than or equal to 4.5g/cm3。
Step five: and carrying out batch processing to obtain the required amorphous nano soft magnetic alloy powder.
Comparative example two:
the preparation method of the amorphous nano magnetically soft alloy powder in the comparative example comprises the following specific steps:
the method comprises the following steps: alloy smelting, wherein the alloy powder comprises the following components in percentage by mass: 6.5% Si, 1.7% B, 1.5% Cu, 5.8% Nb, 0.5% P, and the balance Fe. The method comprises the steps of proportioning according to alloy components, selecting industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus with the purity of 99.9 percent as raw materials, adding the alloy raw materials into a corundum crucible, controlling the smelting power to be 250KW, smelting for 70 minutes, carrying out slagging and deoxidation treatment on molten steel by adopting a proper amount of calcium silicate and lime when the temperature of the molten steel reaches 1500 ℃, reducing the power to be 120KW, and carrying out slagging-off and deoxidation treatment on the molten steel for 10 minutes, then completely slagging off, and pouring steel. Wherein the smelting adopts medium frequency induction smelting.
Step two: performing gas-jet water-cooling atomization to prepare powder, namely preparing powder by adopting an HK-03 annular hole type supersonic gas atomization nozzle, wherein the inner diameter of a leakage pipe of a tundish is 5.5mm, the atomization pressure is 4MPa, and performing water-powder separation and vacuum drying on powder obtained by atomization to obtain a required amorphous powder precursor;
step three: performing crystallization annealing treatment, namely performing crystallization annealing treatment on the atomized amorphous powder at 500 ℃ for 60min by using high-purity hydrogen with the dew point of-60 ℃ as protective atmosphere to obtain amorphous/nanocrystalline magnetically soft alloy powder;
step four: powder grading and screening, wherein the powder granularity and distribution are controlled by air classification, and the powder laser granularity D50 is controlled: 13-17 μm. Powder laser particle size D50: 13-17 μm, oxygen content of powder is less than or equal to 0.1 wt%, and tap density of powder is more than or equal to 4.5g/cm3。
Step five: and carrying out batch processing to obtain the required amorphous nano soft magnetic alloy powder.
Comparative example three:
the preparation method of the amorphous nano magnetically soft alloy powder in the comparative example comprises the following specific steps:
the method comprises the following steps: alloy smelting, wherein the alloy powder comprises the following components in percentage by mass: 6.5% Si, 1.7% B, 1.5% Cu, 5.8% Nb, 0.5% P, and the balance Fe. The method comprises the steps of proportioning according to alloy components, selecting industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus with the purity of 99.9 percent as raw materials, adding the alloy raw materials into a corundum crucible, controlling the smelting power to be 250KW, smelting for 70 minutes, carrying out slagging and deoxidation treatment on molten steel by adopting a proper amount of calcium silicate and lime when the temperature of the molten steel reaches 1500 ℃, reducing the power to be 120KW, and carrying out slagging-off and deoxidation treatment on the molten steel for 10 minutes, then completely slagging off, and pouring steel. Wherein the smelting adopts medium frequency induction smelting.
Step two: performing gas-jet water-cooling atomization to prepare powder, namely preparing powder by adopting an HK-03 annular hole type supersonic gas atomization nozzle, wherein the inner diameter of a leakage pipe of a tundish is 5.5mm, the atomization pressure is 10MPa, and performing water-powder separation and vacuum drying on powder obtained by atomization to obtain a required amorphous powder precursor;
step three: performing crystallization annealing treatment, namely performing crystallization annealing treatment on the atomized amorphous powder at 500 ℃ for 60min by using high-purity hydrogen with the dew point of-60 ℃ as protective atmosphere to obtain amorphous/nanocrystalline magnetically soft alloy powder;
step four: powder grading and screening, wherein the powder granularity and distribution are controlled by air classification, and the powder laser granularity D50 is controlled: 13-17 μm. Powder laser particle size D50: 13-17 μm, oxygen content of powder is less than or equal to 0.1 wt%, and tap density of powder is more than or equal to 4.5g/cm3。
Step five: and carrying out batch processing to obtain the required amorphous nano soft magnetic alloy powder.
Comparative example four:
the preparation method of the amorphous nano magnetically soft alloy powder in the comparative example comprises the following specific steps:
the method comprises the following steps: alloy smelting, wherein the alloy powder comprises the following components in percentage by mass: 6.5% Si, 1.7% B, 1.5% Cu, 5.8% Nb, 0.5% P, and the balance Fe. The method comprises the steps of proportioning according to alloy components, selecting industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus with the purity of 99.9 percent as raw materials, adding the alloy raw materials into a corundum crucible, controlling the smelting power to be 250KW, smelting for 70 minutes, carrying out slagging and deoxidation treatment on molten steel by adopting a proper amount of calcium silicate and lime when the temperature of the molten steel reaches 1500 ℃, reducing the power to be 120KW, and carrying out slagging-off and deoxidation treatment on the molten steel for 10 minutes, then completely slagging off, and pouring steel. Wherein the smelting adopts medium frequency induction smelting.
Step two: performing gas-jet water-cooling atomization to prepare powder, namely preparing powder by adopting an HK-03 annular hole type supersonic gas atomization nozzle, wherein the inner diameter of a leakage pipe of a tundish is 4.0mm, the atomization pressure is 6MPa, and performing water-powder separation and vacuum drying on powder obtained by atomization to obtain a required amorphous powder precursor;
step three: performing crystallization annealing treatment, namely performing crystallization annealing treatment on the atomized amorphous powder at 500 ℃ for 60min by using high-purity hydrogen with the dew point of-60 ℃ as protective atmosphere to obtain amorphous/nanocrystalline magnetically soft alloy powder;
step four: powder grading and screening, wherein the powder granularity and distribution are controlled by air classification, and the powder laser granularity D50 is controlled: 13-17 μm. Powder laser particle size D50: 13-17 μm, oxygen content of powder is less than or equal to 0.1 wt%, and tap density of powder is more than or equal to 4.5g/cm3。
Step five: and carrying out batch processing to obtain the required amorphous nano soft magnetic alloy powder.
Comparative example five:
the preparation method of the amorphous nano magnetically soft alloy powder in the comparative example comprises the following specific steps:
the method comprises the following steps: alloy smelting, wherein the alloy powder comprises the following components in percentage by mass: 6.5% Si, 1.7% B, 1.5% Cu, 5.8% Nb, 0.5% P, and the balance Fe. The method comprises the steps of proportioning according to alloy components, selecting industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus with the purity of 99.9 percent as raw materials, adding the alloy raw materials into a corundum crucible, controlling the smelting power to be 250KW, smelting for 70 minutes, carrying out slagging and deoxidation treatment on molten steel by adopting a proper amount of calcium silicate and lime when the temperature of the molten steel reaches 1500 ℃, reducing the power to be 120KW, and carrying out slagging-off and deoxidation treatment on the molten steel for 10 minutes, then completely slagging off, and pouring steel. Wherein the smelting adopts medium frequency induction smelting.
Step two: performing gas-jet water-cooling atomization to prepare powder, namely preparing powder by adopting an HK-03 annular hole type supersonic gas atomization nozzle, wherein the inner diameter of a leakage pipe of a tundish is 7.0mm, the atomization pressure is 6MPa, and performing water-powder separation and vacuum drying on powder obtained by atomization to obtain a required amorphous powder precursor;
step three: performing crystallization annealing treatment, namely performing crystallization annealing treatment on the atomized amorphous powder at 500 ℃ for 60min by using high-purity hydrogen with the dew point of-60 ℃ as protective atmosphere to obtain amorphous/nanocrystalline magnetically soft alloy powder;
step four: powder grading and screening, wherein the powder granularity and distribution are controlled by air classification, and the powder laser granularity D50 is controlled: 13-17 μm. Powder laser particle size D50: 13-17 μm, oxygen content of powder is less than or equal to 0.1 wt%, and tap density of powder is more than or equal to 4.5g/cm3。
Step five: and carrying out batch processing to obtain the required amorphous nano soft magnetic alloy powder.
Comparative example six:
the preparation method of the amorphous nano magnetically soft alloy powder in the comparative example comprises the following specific steps:
the method comprises the following steps: alloy smelting, wherein the alloy powder comprises the following components in percentage by mass: 6.5% Si, 1.7% B, 0.5% P, and the balance Fe. The method comprises the steps of proportioning according to alloy components, selecting industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus with the purity of 99.9 percent as raw materials, adding the alloy raw materials into a corundum crucible, controlling the smelting power to be 250KW, smelting for 70 minutes, carrying out slagging and deoxidation treatment on molten steel by adopting a proper amount of calcium silicate and lime when the temperature of the molten steel reaches 1500 ℃, reducing the power to be 120KW, and carrying out slagging-off and deoxidation treatment on the molten steel for 10 minutes, then completely slagging off, and pouring steel. Wherein the smelting adopts medium frequency induction smelting.
Step two: performing gas-jet water-cooling atomization to prepare powder, namely preparing powder by adopting an HK-03 annular hole type supersonic gas atomization nozzle, wherein the inner diameter of a leakage pipe of a tundish is 5.5mm, the atomization pressure is 6MPa, and performing water-powder separation and vacuum drying on powder obtained by atomization to obtain a required amorphous powder precursor;
step three: performing crystallization annealing treatment, namely performing crystallization annealing treatment on the atomized amorphous powder at 500 ℃ for 60min by using high-purity hydrogen with the dew point of-60 ℃ as protective atmosphere to obtain amorphous/nanocrystalline magnetically soft alloy powder;
step four: classifying and sieving the powder, controlling the granularity and distribution of the powder by air classification, and controlling the powder excitationLight particle size D50: 13-17 μm. Powder laser particle size D50: 13-17 μm, oxygen content of powder is less than or equal to 0.1 wt%, and tap density of powder is more than or equal to 4.5g/cm3。
Step five: and carrying out batch processing to obtain the required amorphous nano soft magnetic alloy powder.
The powder prepared by the four groups of embodiments and the six groups of embodiments in proportion is used for preparing the magnetic ring inductance element, and the specific process is as follows:
the method comprises the following steps: coating the amorphous nano magnetically soft alloy powder with 1 wt% of KH-550 silane coupling agent and 2 wt% of DC-805 silicone resin, granulating on a granulator to obtain particles with the fineness of 40 meshes, and baking for 1h at 100 ℃;
step two: and (3) taking 27g of the granulation powder obtained after drying in the step one, maintaining the pressure for 3s under the pressure of 1200MPa, and performing cold pressing to obtain the required magnetic ring inductor with the specification of 27mm of outer diameter phi and 14.5mm of inner diameter phi.
XRD diffraction is carried out on the powder prepared in the first embodiment and the conventional amorphous powder to form an XRD diffraction pattern, as shown in figure 1, the powder in the first embodiment is a diffraction pattern positioned above; the conventional amorphous powder is a diffraction pattern positioned below. As shown in fig. 2 and fig. 3, the SEM morphologies of the metal powder in the first example and the first comparative example are shown, respectively, wherein it can be seen that the alloy powder obtained in the first example has good sphericity, high tap density, and good powder dispersibility.
Powder laser granularity, oxygen content and tap density of the powder prepared in the four groups of examples and the six groups of comparative examples are tested, the inductance Ls of the inductance of the magnetic ring is tested by a TH2816B/TH2826LCR tester under the conditions that f is 100kHz and 1V, and the loss value of the inductance of the magnetic ring is tested by an MATS-2010SA soft magnetic alloy alternating-current measuring device under the conditions that Bm is 100T and f is 100 kHz. The specific data are as follows:
TABLE 1 test data for powder, magnetic ring inductors made from various sets of examples and comparative examples
It can be known from table 1 that the gas-jet water-cooling atomization powder preparation process is adopted, and the characteristics of reasonable particle size distribution, good powder sphericity, high tap density, low oxygen content and the like of the prepared soft magnetic alloy powder are better ensured by optimally designing the inner diameter of the leakage pipe of the tundish and the atomization pressure, and the prepared magnetic ring inductance part product has good pressing performance, high inductance value and permeability and low loss. The addition of a small amount of Cu and Nb elements plays a vital role in the nucleation of the nanocrystalline and the inhibition of the precipitation of a primary crystal phase in the crystallization process of the alloy, so that the growth of alpha-Fe (Si) phase grains is prevented, and the amorphous nanocrystalline material has better comprehensive performance.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the amorphous nano magnetically soft alloy powder is characterized in that the obtained alloy powder comprises the following components in percentage by mass: 6-9% of Si, 1-2.5% of B, 1-3% of Cu, 4-7% of Nb, 0.5-2% of P and 82-87.5% of Fe.
2. The method for preparing amorphous nano magnetically soft alloy powder according to claim 1, wherein the obtained alloy powder comprises the following components in percentage by mass: 6.5% Si, 1.7% B, 1.5% Cu, 5.8% Nb, 0.5% P, and the balance Fe.
3. The method for preparing amorphous nano soft magnetic alloy powder according to claim 1, comprising the steps of:
the method comprises the following steps: smelting an alloy, burdening according to alloy components, selecting industrial pure iron, pure copper, industrial ferroboron, monocrystalline silicon, ferroniobium and ferrophosphorus with the purity of 99.9 percent as raw materials, and adding the alloy raw materials into a corundum crucible for steel burning;
step two: performing gas-jet water-cooling atomization to prepare powder, and performing water-powder separation and vacuum drying on powder obtained by atomization by adopting a supersonic gas atomization nozzle to obtain a required amorphous powder precursor;
step three: performing crystallization annealing treatment, namely performing crystallization annealing treatment on atomized amorphous powder at 500-600 ℃ for 60-90min by using high-purity hydrogen with the dew point of-60 ℃ as protective atmosphere to obtain amorphous/nanocrystalline magnetically soft alloy powder;
step four: powder grading and screening, wherein the powder granularity and distribution are controlled by air classification, and the powder laser granularity D50 is controlled: 13-17 μm.
Step five: and carrying out batch processing to obtain the required amorphous nano soft magnetic alloy powder.
4. The method for preparing amorphous nano magnetically soft alloy powder according to claim 3, wherein in the second step, an annular supersonic gas atomizing nozzle is adopted, the inner diameter of a tundish leakage pipe is 5.0-6.0mm, and the atomizing pressure is 6-8 MPa.
5. The method for preparing amorphous nano magnetically soft alloy powder according to claim 4, wherein the ring-hole type supersonic gas atomizing nozzle is HK-03 type.
6. The method for preparing amorphous nano magnetically soft alloy powder as claimed in claim 5, wherein in the step one, the smelting power is controlled to be 200-plus 300KW, the smelting time is 60.0-80.0 minutes, when the temperature of the molten steel reaches 1500-plus 1520 ℃, the power is reduced to be 100-plus 150KW, a proper amount of calcium silicon and lime are adopted to carry out slagging and deoxidation treatment on the molten steel, the process time is 10.0-15.0 minutes, then the slag is completely removed, and the steel is poured.
7. The method for preparing amorphous nano magnetically soft alloy powder according to claim 6, wherein the laser particle size of the powder in step four is D50: 13-17 μm, oxygen content of powder is less than or equal to 0.1 wt%, and tap density of powder is more than or equal to 4.5g/cm 3.
8. An amorphous nano soft magnetic alloy powder, characterized by being prepared by the preparation method of any one of claims 1 to 7.
9. A preparation method of a magnetic ring inductor is characterized by comprising the following steps:
the method comprises the following steps: coating the amorphous nano soft magnetic alloy powder of claim 8 by 1 wt% of KH-550 silane coupling agent and 2 wt% of DC-805 silicone resin, granulating on a granulator to obtain particles with the fineness of 40 meshes, and baking for 1h at 100 ℃;
step two: and (3) taking 27g of the granulation powder obtained after drying in the step one, maintaining the pressure for 3s under the pressure of 1200MPa, and performing cold pressing to obtain the required magnetic ring inductor.
10. A magnetic ring inductor, characterized in that, it is made by the preparation method of claim 9, and its specification is 27mm of outside diameter phi x 14.5mm of inside diameter phi; f is 100kHz, under the condition of 1V, the inductance value Ls of the magnetic ring is more than or equal to 60 mu H, the magnetic conductivity mu is more than or equal to 50, the loss Ps is less than or equal to 500kW/m3。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010720769.6A CN111968821A (en) | 2020-07-24 | 2020-07-24 | Soft magnetic alloy powder and preparation method thereof, and magnetic ring inductor and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010720769.6A CN111968821A (en) | 2020-07-24 | 2020-07-24 | Soft magnetic alloy powder and preparation method thereof, and magnetic ring inductor and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN111968821A true CN111968821A (en) | 2020-11-20 |
Family
ID=73362588
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202010720769.6A Pending CN111968821A (en) | 2020-07-24 | 2020-07-24 | Soft magnetic alloy powder and preparation method thereof, and magnetic ring inductor and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN111968821A (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112743094A (en) * | 2020-12-29 | 2021-05-04 | 南通金源智能技术有限公司 | Preparation method and device of novel superfine amorphous magnetic powder |
CN112846180A (en) * | 2021-01-05 | 2021-05-28 | 北京科技大学 | Method for preparing high-magnetic-performance phosphorus-containing silicon steel sheet through powder sintering |
CN114045435A (en) * | 2021-11-11 | 2022-02-15 | 泉州天智合金材料科技有限公司 | Iron-based amorphous nanocrystalline wave-absorbing material and preparation method thereof |
CN114147212A (en) * | 2020-11-30 | 2022-03-08 | 佛山市中研非晶科技股份有限公司 | Amorphous nanocrystalline atomized powder and preparation method thereof |
CN114260457A (en) * | 2021-01-15 | 2022-04-01 | 武汉科技大学 | FeSiBCCr amorphous magnetic powder and preparation method thereof |
CN114309628B (en) * | 2021-01-15 | 2024-07-09 | 武汉科技大学 | FeSiBPNbCr amorphous magnetic powder and preparation method thereof |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104475743A (en) * | 2014-11-25 | 2015-04-01 | 北京康普锡威科技有限公司 | Manufacturing method of micro spherical titanium and titanium alloy powder |
CN104934179A (en) * | 2014-05-27 | 2015-09-23 | 安泰科技股份有限公司 | Fe-based nanocrystalline soft magnetic alloy with strong amorphous forming ability and preparing method of Fe-based nanocrystalline soft magnetic alloy |
WO2017086102A1 (en) * | 2015-11-17 | 2017-05-26 | アルプス電気株式会社 | Method of producing dust core |
CN109877311A (en) * | 2019-04-17 | 2019-06-14 | 泉州天智合金材料科技有限公司 | A kind of MIM is injection moulded high-end cutter, metal powder and preparation method thereof |
CN111246952A (en) * | 2017-08-07 | 2020-06-05 | 日立金属株式会社 | Crystalline Fe-based alloy powder and method for producing same |
-
2020
- 2020-07-24 CN CN202010720769.6A patent/CN111968821A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104934179A (en) * | 2014-05-27 | 2015-09-23 | 安泰科技股份有限公司 | Fe-based nanocrystalline soft magnetic alloy with strong amorphous forming ability and preparing method of Fe-based nanocrystalline soft magnetic alloy |
CN104475743A (en) * | 2014-11-25 | 2015-04-01 | 北京康普锡威科技有限公司 | Manufacturing method of micro spherical titanium and titanium alloy powder |
WO2017086102A1 (en) * | 2015-11-17 | 2017-05-26 | アルプス電気株式会社 | Method of producing dust core |
CN111246952A (en) * | 2017-08-07 | 2020-06-05 | 日立金属株式会社 | Crystalline Fe-based alloy powder and method for producing same |
CN109877311A (en) * | 2019-04-17 | 2019-06-14 | 泉州天智合金材料科技有限公司 | A kind of MIM is injection moulded high-end cutter, metal powder and preparation method thereof |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114147212A (en) * | 2020-11-30 | 2022-03-08 | 佛山市中研非晶科技股份有限公司 | Amorphous nanocrystalline atomized powder and preparation method thereof |
CN112743094A (en) * | 2020-12-29 | 2021-05-04 | 南通金源智能技术有限公司 | Preparation method and device of novel superfine amorphous magnetic powder |
CN112846180A (en) * | 2021-01-05 | 2021-05-28 | 北京科技大学 | Method for preparing high-magnetic-performance phosphorus-containing silicon steel sheet through powder sintering |
CN114260457A (en) * | 2021-01-15 | 2022-04-01 | 武汉科技大学 | FeSiBCCr amorphous magnetic powder and preparation method thereof |
CN114289726A (en) * | 2021-01-15 | 2022-04-08 | 武汉科技大学 | FeSiBPNbCu nanocrystalline magnetic powder and preparation method thereof |
CN114309628A (en) * | 2021-01-15 | 2022-04-12 | 武汉科技大学 | FeSiBPNbCr amorphous magnetic powder and preparation method thereof |
CN114309628B (en) * | 2021-01-15 | 2024-07-09 | 武汉科技大学 | FeSiBPNbCr amorphous magnetic powder and preparation method thereof |
CN114289726B (en) * | 2021-01-15 | 2024-07-09 | 武汉科技大学 | FeSiBPNbCu nanocrystalline magnetic powder and preparation method thereof |
CN114045435A (en) * | 2021-11-11 | 2022-02-15 | 泉州天智合金材料科技有限公司 | Iron-based amorphous nanocrystalline wave-absorbing material and preparation method thereof |
CN115537684A (en) * | 2021-11-11 | 2022-12-30 | 泉州天智合金材料科技有限公司 | Novel iron-based amorphous nanocrystalline wave-absorbing material and preparation method thereof |
CN115537684B (en) * | 2021-11-11 | 2024-04-12 | 泉州天智合金材料科技有限公司 | Novel iron-based amorphous nanocrystalline wave-absorbing material and preparation method thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN111968821A (en) | Soft magnetic alloy powder and preparation method thereof, and magnetic ring inductor and preparation method thereof | |
CN104475742A (en) | Manufacturing method of iron-based amorphous soft magnetic alloy spherical powder | |
CN112105472B (en) | Powder for magnetic core, magnetic core using same, and coil component | |
WO2013157596A1 (en) | PROCESS FOR PRODUCING AMORPHOUS SPRAYED COATING CONTAINING α-Fe NANOCRYSTALS DISPERSED THEREIN | |
TW201917224A (en) | Crystalline fe-based alloy powder and method of producing the same | |
JP2008294411A (en) | Soft magnetism powder, manufacturing method for dust core, dust core, and magnetic component | |
Wu et al. | Evolution from amorphous to nanocrystalline and corresponding magnetic properties of Fe-Si-B-Cu-Nb alloys by melt spinning and spark plasma sintering | |
JP2023544559A (en) | Alloy powder, its manufacturing method, and uses | |
KR20210002498A (en) | Alloy powder, Fe-based nanocrystalline alloy powder and magnetic core | |
CN106756644A (en) | A kind of iron-based amorphous and nanocrystalline soft magnetic alloy based on element silicon and preparation method thereof | |
WO2003012802A1 (en) | Method for producing nanocomposite magnet using atomizing method | |
Larimian et al. | Bulk-nano spark plasma sintered Fe-Si-B-Cu-Nb based magnetic alloys | |
CN110571009A (en) | Iron-based spheroidized micro-nano magnetic powder core and preparation method thereof | |
CN100510114C (en) | Heat treating process for Fe-based big block amorphous alloy crystallization | |
TW201917225A (en) | Fe-based alloy, crystalline fe-based alloy atomized powder, and magnetic core | |
CN116079066A (en) | TaNbTiZr refractory high-entropy alloy spherical powder and preparation method thereof | |
CN111375782B (en) | Preparation method of iron-nickel-molybdenum soft magnetic powder | |
CN113878124A (en) | Water-gas combined atomization preparation method of Fe-Si-Cr-Ga-in-N alloy soft magnetic powder | |
CN103406545A (en) | Preparation method of micron-particle-size FeCo particles | |
JP2018137306A (en) | Soft magnetic powder, magnetic part and powder-compact magnetic core | |
Lei et al. | Fabrication of spherical Fe-based magnetic powders via the in situ de-wetting of the liquid–solid interface | |
Ram | Synthesis, magnetic properties and formalism of magnetic properties of high-quality refined Nd2Fe14B powders for permanent magnet devices | |
CN117809925B (en) | Nanocrystalline magnetic core material of high-frequency transformer and preparation method thereof | |
Nascimento et al. | THE POWDER OF Co64Nb30B6 OBTAINED BY MECHANICAL ALLOYING | |
JP2019090103A (en) | Soft magnetic metal powder, production method thereof and soft magnetic metal dust core |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |