CN103551565A - Manufacturing method for soft-magnetic Fe-Si-Al-Ni alloy powder - Google Patents
Manufacturing method for soft-magnetic Fe-Si-Al-Ni alloy powder Download PDFInfo
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- CN103551565A CN103551565A CN201310524826.3A CN201310524826A CN103551565A CN 103551565 A CN103551565 A CN 103551565A CN 201310524826 A CN201310524826 A CN 201310524826A CN 103551565 A CN103551565 A CN 103551565A
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Abstract
A manufacturing method for soft-magnetic Fe-Si-Al-Ni alloy powder comprises smelting alloy formed by 4.0% to 5.0% of Si, 3.0% to 4.0% of Al, 1.0% to 2.5% of Ni, 0.1% to 0.4% of Ti, 0.1% to 0.4% of Mn, 0.1% to 0.5% of P, 0.02% or less of C, and the balance Fe through an induction heating vacuum rapid solidification furnace, performing rapid solidification on the alloy to manufacture sheet materials, and subjecting the sheet materials to mechanical crushing, thermal processing of crushed materials, ball milling of the materials into fine powder, annealing treatment and screening and particle size distribution. The method has the advantages that the smelting alloy material is pure, the alloy saturation induction density Bs is more than 18000 gausses, and the adding of Ni can guarantee that the alloy magnetostriction coefficient is zero; excellent soft magnetic properties are provided during magnetic powder core manufacturing, and the AC/DC superposition performance is good particularly when the magnetic conductivity of pressed products is mu e60, for example, when AC is 100 KHz, DCH is equal to 50 Oe, mu 50 >=88% mu O, and the magnetic core loss is lower than that of the high-flux Fe50 Ni50 magnetic powder core, so that the soft-magnetic Fe-Si-Al-Ni alloy powder can replace Fe50 Ni50 and Fe-Si alloy magnetic powder cores to be used in electronic and electric industries.
Description
Technical field
The invention belongs to the manufacture method of magnetic bodies---particularly there is the manufacture method of the iron, silicon, aluminum and nickel alloy powder of soft magnetic characteristic.
Background technology
In recent years, along with scientific and technological progress, to environmental protection, the raising of energy-conservation requirement, impel electronics, electric utility is to miniaturization, high efficiency direction conducts a research and develops, soft magnetic metal powder core receives great concern, because the electronic devices and components of making for this kind of material have energy storage, the function of electromagnetic conversion, concrete application is production control, the Switching Power Supply of conversion, the iron nickel system alloy powder core of early application, due to the high restriction that is subject to market of its price, find new inexpensive material, use in a large number subsequently straight iron powder core, but its magnetic conductivity is low, core loss large (easily heating), be subject to the restriction of some occasions, the sendust of early detection, owing to smelting composition, be difficult to control, be subject to the cold reception of long term, improvement through smelting technique, improve, nearly ten years, Fe-Si-Al magnetic core is paid attention to widely and is applied, can replace within the specific limits nickelic permalloy (MPP) powder core.Electronics, electric utility require saturation induction density Bs value higher, and alternating current-direct current additivity can better functional material.The Bs value of finding Fe-6.5Si alloy can reach 15000 Gausses, its electromagnetic performance can approach the requirement of Fe50 Ni50 alloy magnetic powder core, be subject to vast magnetics researcher's attention, further find that super celestial platform alloy (Si6-Al4-Ni3.2 alloy) is as more superior than the electromagnetic performance of Fe-6.5Si alloy in μ e60 at low magnetic permeability.But iron-nickel alloy (Ni81 Mo2, Fe50 Ni50) and ferro-silicium (Fe-6.5Si, FeSi6 Al4 Ni3.2) powder process only can be produced with atomization, the atomized powder of ferro-silicium insufficient formability when making stampings thereafter particularly, the core loss of the stampings of water atomization powder (powder core) is large, and the cost of aerosolization powder is high.
The present invention studies near the component of super celestial platform alloy, adjusting component, add favourable alloying element, high saturation induction density Bs value has more than can reach 18000 Gausses, low coercivity H≤0.2Oe, the thin slice material that rapid hardening throws away can add the alloy powder that ball-milling technology is made by Mechanical Crushing, makes the technique of magnetic, can simplify, the electromagnetic performance of its powder compaction product is all better than iron silica magnetic particle core and Fe50 Ni50 powder core.
Summary of the invention
The object of the invention is to study the manufacture method of the alloy powder that a kind of novel metal soft-magnetic powder core uses.Its emphasis gets rid of flakiness shape by eddy-current heating vacuum rapid hardening method, after fragmentation, ball milling, heat treatment, produce for pressed magnetic powder core alloy powder, there is good moldability, core loss is low, the good feature of alternating current-direct current stack performance, the powder that can replace atomization to make.The electromagnetic property of the powder core making with the powder that this method is produced, reaches Fe50ni50 perm and closes the level with ferro-silicium.For example manufacture the powder core of magnetic conductivity μ e60, have low magnetic Job's tears power attenuation, be less than 600mw/cm3 when frequency 50kHz magnetic field 1000Gs, alternating current-direct current stack performance exchanges Ac100kH
2, direct current DC, during magnetic field H=50Oe, μ e50>=88% μ o.μ o is the magnetic conductivity without D.C. magnetic field.
The manufacture method of iron, silicon, aluminum and nickel alloy powder of the present invention, comprises the steps:
1, by eddy-current heating vacuum rapid hardening furnace alloy smelting rapid hardening flakiness shape material---Mechanical Crushing---broken material heat treatment---ball milling becomes fine powder---annealing in process.It is characterized in that:
A) mass percentage content of alloy component is Si 4.0～5.0%, and Al 3.0～4.0%, and Ni 1.0～2.5%, Ti 0.1～.4%, and Mn 0.1～0.4%, and P 0.1～0.5%, C≤0.02%, remaining is Fe;
B) raw material that adopt are ingot irons, polysilicon, fine aluminium, pure nickel, titanium sponge and manganese metal, ferrorphosphorus;
2, Mechanical Crushing particle is 3-10mm, adopts hydrogen shield heat treatment, and temperature is 900-1150 ℃, temperature retention time 2-4 hour;
3, the particulate material after heat treatment is worn into-100 order powder with ball tube mill tool or ring-roller mill, carries out nitrogen formula protection heat treatment, and temperature is 800-950 ℃, is incubated 2-6 hours.
The manufacture method of the iron, silicon, aluminum and nickel alloy powder of soft magnetic characteristic of the present invention, its advantage is as follows:
1) Main Ingredients and Appearance due to alloy powder is that Fe Si Al Ni forms the saturation induction density Bs value (the Bs value of Fe50 Ni50 and Fe-6.5si is about 15000 Gausses) more than 18000 Gausses that has guaranteed alloy, added a small amount of P, Ti, Mn element, improved the broken ball milling performance of alloy, and the magnetic hystersis loss of alloy and eddy-current loss are reduced.
2) with eddy-current heating vacuum rapid hardening, producing thin slice material, is first to make alloy sublimate, has simplified Mechanical Crushing ball-milling technology simultaneously, and the processing performance that makes powder is better than the powder of producing with atomization.With the powder shape that the method is produced, be particularly polygon, its post-production stampings are better than spherical mouldability and the compressibility of atomization.
3) twice heat treated benefit is first to have adjusted the inner phase structure of alloy, forms ordering extra-structure (Fe3 Si Al, Fe Si Al), after be the mechanical stress of eliminating Mechanical Crushing, the coercivity of powder is reduced.
The specific embodiment
embodiment mono-:
1) with nominal 500kg eddy-current heating vacuum rapid hardening furnace alloy smelting.By ingot iron, polysilicon, fine aluminium, pure nickel, manganese metal, ferrorphosphorus and titanium sponge, drop into by a certain percentage in stove and smelt, and under vacuum protection rapid hardening flakiness shape.The mass percentage content of its chemical composition is: Si4.50%, and Al4.0%, Ni1.50%, P0.30%, Mn0.20%, Ti0.40%, C0.012%, O280PPm, N230PPm is remaining is Fe;
2) above-mentioned alloy sheet is broken into 3-10mm particle sheet stock with mechanical crushing method;
3) will make particle sheet stock and carry out hydrogen shield heat treatment, temperature is 1050 ℃, is incubated 3 hours;
4), by the particle sheet stock after heat treatment, drop into the fine powder material that ball mill is worn into-100 orders (< 150 μ m);
5) above-mentioned fine powder material is carried out to nitrogen protection heat treatment, temperature is 800 ℃, is incubated 6 hours;
6) electromagnetic performance of alloy: initial permeability μ o is 2500 Gausses/oersted, maximum permeability μ m is that 18350 Gs/Oe coercivity H are 0.18Oe, and resistance coefficient ρ is 66 μ Ω cm, and saturation induction density Bs is 18800Gs;
The magnetic property of alloy powder: coercivity jHc1.26Oe, specific saturation magnetization Ms190.0emu/g, than remanent magnetization Mr0.12 emu/g, vibrating example magnetic strength instrument (VSM) test.
Domestic Fe-6.5si aerosolization powder: jHe3.18Oe, Ms168.8emu/g, Mr0.28emu/g.
embodiment bis-
1) smelting of alloy and make thin slice material, with 1 of embodiment mono-, the mass percentage content of the chemical composition of alloy is: Si5.0%, Al3.0%, Ni1.50%, P0.50%, Mn0.40%, Ti0.10%, C0.010%, O 2BOPPm, N235ppm is remaining is Fe;
2) thin slice material becomes 3-10mm particle sheet stock by Mechanical Crushing;
3) heat treatment of thin slice material is with 3 of embodiment mono-, and heat treatment temperature is 1150 ℃, and temperature retention time is 2 hours;
4) sheet of particles pellet mill is with 4 of embodiment mono-;
5) fine powder material heat treatment is with 5 of embodiment mono-, and nitrogen protection heat treatment temperature is 880 ℃, is incubated 4 hours;
6) electromagnetic performance of alloy: μ o is 2350Gs/oe, μ m is 19500Gs/Oe, and Hc is 0.16Oe, and ρ is 68 μ Ω
., cm.
embodiment tri-
1) alloy smelting and make thin slice material with 1 of embodiment mono-, the percentage of rolling of the chemical composition of alloy containing reason is: Si4.0%, Al3.5%, Ni1.50%, P0.10%, Mn0.10%, Ti0.25%, C0.008%, O
280ppm, N
230ppm, remaining is Fe;
2) thin slice material is broken into 3-10mm particle sheet stock by Mechanical Method;
3) particle sheet stock heat treatment hydrogen shield, temperature is 950 ℃, is incubated 2 hours;
4), by the particle sheet stock after processing, drop into ball mill and wear into-100 object fine powder materials;
5) will carry out nitrogen protection heat treatment to fine powder material, temperature is 900 ℃, and the time is 4 hours;
6) electromagnetic performance of alloy; μ
0for 2400Gs/Oe, μ m is 19000Gs/Oe, and Hc is 0.15Oe, and ρ is 70 μ Ω cm.
The magnetic property of alloy powder: jHc 1.14Oe, Ms 190.0emu/g, Mr 0.12 emu/g.
embodiment tetra-
In order to verify the making electronic devices and components (inductance component such as powder core, annular, square, E type) of soft-magnetic alloy powder, must make powder core and detect its electromagnetic performance, as magnetic conductivity, alternating current-direct current stack performance, core loss, can compare it simultaneously and make powder processing performance.The compressing powder core of take below describes as example.
1) alloy powder of embodiment mono-～embodiment tri-is pressed to following granularmetric composition, its mass percentage content is :-100～+ 200 order≤5% ,-200～+ 300 orders account for 45～50%, and remaining is-300 orders.
2) with the alloy powder of the above-mentioned granularmetric composition of phosphoric acid,diluted solution immersion, make its powder surface form dielectric film, add appropriate insulating compound (as kaolin or mica powder), lubricant, releasing agent, stir and become compacting powder.
3) above-mentioned powder is dropped into dry powder automatic forming press and suppress, pressure is that 22-24T/cm2 is pressed into annular, and compacting specification is external diameter φ 26.90mm, internal diameter φ 14.70mm, and height 11.20mm, stampings density is 6.8-7.0g/cm3.
4) stampings are heat-treated with nitrogen protection, and temperature is 700-720 ℃, is incubated 1 hour.
5) detecting its magnetic parameter sees the following form:
Claims (3)
1. a manufacture method for iron, silicon, aluminum and nickel alloy powder, comprising: with eddy-current heating vacuum rapid hardening furnace alloy smelting rapid hardening flakiness shape material-Mechanical Crushing-broken material heat treatment-ball milling, become fine powder-annealing in process, it is characterized in that:
1. the mass percent of alloy component is: Si 4.0～5.0%, Al 3.0～4.0%, Ni 1.0～2.5%, Ti 0.1～0.4%, Mn 0.1～0.4%, P 0.1～0.5%, C≤0.02%, and remaining is Fe;
2. the raw material that adopt are ingot iron, polysilicon, fine aluminium, pure nickel, titanium sponge and manganese metal, ferrorphosphorus.
2. the manufacture method of a kind of iron, silicon, aluminum and nickel alloy powder according to claim 1, is characterized in that: Mechanical Crushing particle is 3-10mm: adopt hydrogen shield heat treatment, temperature is 900-1150 ℃, temperature retention time 2-4 hour.
3. the manufacture method of a kind of iron, silicon, aluminum and nickel alloy powder according to claim 2; it is characterized in that: the particulate material after described heat treatment, with cartridge type ball milling or ring-roller mill, wear into-100 order powder, carry out nitrogen protection heat treatment; temperature is 800-950 ℃, insulation 2-6 hour.
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| CN103996479A (en) * | 2014-05-22 | 2014-08-20 | 吴娟 | Manufacturing method of sendust core with magnetic permeability mue 200 |
| CN105970083A (en) * | 2016-06-06 | 2016-09-28 | 古前春 | Manufacturing process for iron-silicon-aluminum alloy powder |
| CN111531172A (en) * | 2020-05-29 | 2020-08-14 | 同济大学 | 3D printing process method of high-strength aluminum-silicon alloy |
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| CN111531172A (en) * | 2020-05-29 | 2020-08-14 | 同济大学 | 3D printing process method of high-strength aluminum-silicon alloy |
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