CN103551565B

CN103551565B - The manufacture method of soft magnet silicon, aluminum and nickel alloy powder

Info

Publication number: CN103551565B
Application number: CN201310524826.3A
Authority: CN
Inventors: 刘善宜; 祝家贵; 刘志文; 王�锋
Original assignee: WUHAN XINDA MAGNETISM MATERIAL CO Ltd
Current assignee: WUHAN XINDA MAGNETISM MATERIAL CO Ltd
Priority date: 2013-10-30
Filing date: 2013-10-30
Publication date: 2016-08-17
Anticipated expiration: 2033-10-30
Also published as: CN103551565A

Abstract

A kind of manufacture method of iron, silicon, aluminum and nickel alloy powder, including: sensing heating, vacuum rapid hardening furnace is smelted, 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%, remaining be the alloy of Fe, and rapid hardening material Mechanical Crushing broken material heat treatment ball milling of laminating becomes fine powder annealing sub-sieve grain size proportion.This kind of powder is mainly used for making the iron core of the iron inductance of electronic devices and components, referred to as alloy magnetic powder core.Its advantage is that alloy smelting material is pure, and the saturation induction density Bs value of alloy is more than 18000 Gausses, and interpolation nickel element can ensure that the magnetostriction coefficient of alloy is zero.When having the magnetic permeability μ e60 of excellent soft magnetic characteristic, particularly stampings when manufacturing powder core, alternating current-direct current superposition performance is good, during such as AC 100KHz, DC, H=50Oe, and μ e50 >=88% μ_oAbove, core loss is less than high flux Fe50 Ni50 powder core, can substitute for Fe50 Ni50 and ferrum-silicon alloy magnetic powder core in electronics, electric utility application.

Description

The manufacture method of soft magnet silicon, aluminum and nickel alloy powder

Technical field

The invention belongs to the manufacture method that the manufacture method of magnetic bodies particularly has the iron, silicon, aluminum and nickel alloy powder of soft magnetic characteristic.

Background technology

nullIn recent years，Progress along with science and technology，To environmental protection、The raising of power conservation requirement，Promote electronics、Electric utility is to miniaturization、High efficiency direction conducts a research and develops，Metal soft magnetic powder core is paid close attention to greatly，Because the electronic devices and components that this kind of material is made have energy storage、The function of electromagnetic conversion，Concrete application is to manufacture control、The Switching Power Supply of conversion，The ferrum nickel system alloy powder core of early application，Owing to its price height is restricted by market，Find new inexpensive material，Use straight iron powder core the most in a large number，But its pcrmeability is low、Core loss big (easily heating)，Limited by some occasions，The sendust of early discovery，It is difficult to control to owing to smelting composition，Cold reception by the long term，Improvement through smelting technique、Improve，Nearly ten years，Fe-Si-Al magnetic core is paid attention to widely and is applied，Nickelic permalloy (MPP) powder core can be replaced within the specific limits.Electronics, electric utility require that saturation induction density Bs value is higher, the more preferable functional material of alternating current-direct current superposition performance.The Bs value of discovery Fe-6.5Si alloy is up to 15000 Gausses, and its electromagnetic performance can be close to Fe₅₀Ni₅₀Alloy magnetic powder core requirement, is paid attention to by vast magnetics researcher, it has further been found that super celestial platform alloy (Si6-Al4-Ni3.2 alloy) is more superior than the electromagnetic performance of Fe-6.5Si alloy at low magnetic permeability such as μ e60.But iron-nickel alloy (Ni₈₁Mo₂, Fe₅₀Ni₅₀) and ferro-silicium (Fe-6.5Si, FeSi6Al4Ni3.2) powder process is only capable of producing with atomization, insufficient formability when particularly the atomized powder of ferro-silicium makes stampings behind, the core loss of the stampings (powder core) of water atomized powders is big, 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, have high saturation induction density Bs value up to 18000 Gausses more than, low coercivity H≤0.2Oe, the thin slice material that rapid hardening throws away can add, by Mechanical Crushing, the alloy powder that ball-milling technology is made, the technique making magnetic powder, can simplify, the electromagnetic performance of its powder stampings is superior to ferrum silica magnetic particle core and Fe₅₀N_i50Powder core.

Summary of the invention

It is an object of the invention to study the manufacture method of the alloy powder of a kind of novel metal soft-magnetic powder core.Its emphasis sensing heating, vacuum rapid hardening method gets rid of flakiness shape, produce after broken, ball milling, heat treatment for pressed magnetic powder core alloy powder, there is good moldability, core loss is low, the feature that alternating current-direct current superposition performance is good, can substitute for the powder that atomization prepares.The electromagnetic property of the powder core that the powder produced by this method prepares, reaches the level of Fe50ni50 permalloy and ferro-silicium.Such as manufacture the powder core of magnetic permeability μ e60, there is low magnetic Job's tears power attenuation, when frequency 50kHz magnetic field 1000Gs less than 600mw/cm³, alternating current-direct current superposition performance exchange Ac100kHz, direct current DC, during the H=50Oe of magnetic field, μ e₅₀>=88% μ_o。μ_oFor the pcrmeability without D.C. magnetic field.

The manufacture method of iron, silicon, aluminum and nickel alloy powder of the present invention, comprises the steps:

1, fine powder is become to make annealing treatment with sensing heating, vacuum rapid hardening furnace alloy smelting rapid hardening flakiness shape material Mechanical Crushing broken material heat treatment ball milling.It is characterized in that:

A) mass percentage content of alloy component is Si 4.0～5.0%, Al 3.0～4.0%, Ni 1.0～2.5%, Ti 0.1～.4%, Mn 0.1～0.4%, P 0.1～0.5%, and C≤0.02% is remaining for Fe；

B) raw material used is ingot iron, polysilicon, fine aluminium, pure nickel, titanium sponge and manganese metal, ferrorphosphorus；

2, Mechanical Crushing granule is 3 10mm, uses hydrogen shield heat treatment, and temperature is 900 1150 DEG C, temperature retention time 2-4 hour；

3 ,-100 mesh powder worn into by particulate material ball tube mill tool or ring-roller mill after heat treatment, carry out nitrogen formula protection heat treatment, and temperature is 800 950 DEG C, is incubated 26 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) it is that Fe Si Al Ni composition ensure that saturation induction density Bs value (Fe more than 18000 Gausses of alloy due to the Main Ingredients and Appearance of alloy powder₅₀Ni₅₀It is about 15000 Gausses with the Bs value of Fe-6.5si), with the addition of a small amount of P, Ti, Mn element, improve alloy breaks down ball milling performance, and the magnetic hystersis loss of alloy and eddy-current loss are reduced.

2) producing thin slice material with sensing heating, vacuum rapid hardening, be first so that alloy sublimate, simplify Mechanical Crushing ball-milling technology simultaneously, the processing performance preparing powder is better than the powder with atomization production.The powder shape particularly produced by the method is polygon, and its post-production stampings are better than spherical mouldability and the compressibility of atomization.

3) benefit of twice heat treatment is first to have adjusted the internal phase structure of alloy, forms ordering extra-structure (Fe3 Si Al, Fe Si Al), after be the mechanical stress eliminating Mechanical Crushing so that the coercivity of powder reduces.

Detailed description of the invention

Embodiment one:

1) heating, vacuum rapid hardening furnace alloy smelting is sensed by nominal 500kg.By ingot iron, polysilicon, fine aluminium, pure nickel, manganese metal, ferrorphosphorus and titanium sponge, smelt in putting into stove by a certain percentage, and rapid hardening flakiness shape under vacuum protection.The mass percentage content of its chemical composition is: Si4.50%, Al4.0%, Ni1.50%, P0.30%, Mn0.20%, Ti0.40%, C0.012%, O₂80PPm, N₂30PPm is remaining is Fe；

2) above-mentioned alloy sheet mechanical crushing method is broken into 3 10mm granule sheet stocks；

3) prepared granule sheet stock being carried out hydrogen shield heat treatment, temperature is 1050 DEG C, is incubated 3 hours；

4) by the granule sheet stock after heat treatment, put into ball mill and wear into the fine powder material of 100 mesh (＜ 150 μm)；

5) above-mentioned fine powder material carries out nitrogen protection heat treatment, and temperature is 800 DEG C, is incubated 6 hours；

6) electromagnetic performance of alloy: initial permeability μ o is 2500 Gausses/oersted, maximum permeability μm be 18350Gs/Oe coercivity H be 0.18Oe, 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, ratio remanent magnetization Mr0.12emu/g, vibrating example magnetic strength instrument (VSM) is tested.

Domestic Fe-6.5si aerosolization powder: jHe3.18Oe, Ms168.8emu/g, Mr0.28emu/g.

Embodiment two

1) smelting of alloy and prepared thin slice material, with the 1 of embodiment one, the mass percentage content of the chemical composition of alloy is: Si5.0%, Al3.0%, Ni 1.50%, P0.50%, Mn0.40%, Ti0.10%, C0.010%, O₂BOPPm, N₂35ppm is remaining is Fe；

2) thin slice material Mechanical Crushing becomes 3-10mm granule sheet stock；

3) thin slice material heat treatment is with the 3 of embodiment one, and heat treatment temperature is 1150 DEG C, and temperature retention time is 2 hours；

4) sheet of particles pellet grinds with the 4 of embodiment one；

5) fine powder material heat treatment is with the 5 of embodiment one, and nitrogen protection heat treatment temperature is 880 DEG C, is incubated 4 hours；

6) electromagnetic performance of alloy: μ o is 2350Gs/oe, μm be 19500Gs/Oe, Hc be 0.16Oe, ρ be 68 μ Ω^.,cm。

Embodiment three

1) alloy smelting and prepared thin slice material with the 1 of embodiment one, the percentage ratio of rolling of the chemical composition of alloy containing reason are: Si4.0%, Al3.5%, Ni1.50%, P0.10%, Mn0.10%, Ti0.25%, C0.008%, O₂80ppm, N₂30ppm, remaining for Fe；

2) thin slice material Mechanical Method is broken into 3 10mm granule sheet stocks；

3) granule sheet stock heat treatment hydrogen shield, temperature is 950 DEG C, is incubated 2 hours；

4) the granule sheet stock after processing, puts into ball mill and wears into the fine powder material of 100 mesh；

5) fine powder material will carry out nitrogen protection heat treatment, and temperature is 900 DEG C, and the time is 4 hours；

6) electromagnetic performance of alloy；μ₀For 2400Gs/Oe, μm be 19000Gs/Oe, Hc be 0.15Oe, ρ be 70 μ Ω cm.

The magnetic property of alloy powder: jHc 1.14Oe, Ms 190.0emu/g, Mr 0.12emu/g.

Embodiment four

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, powder core must be made and detect its electromagnetic performance, such as pcrmeability, alternating current-direct current superposition performance, core loss, can be compared it simultaneously and make powder processing performance.Illustrate as a example by compressing powder core below.

1) by the alloy powder of embodiment one～embodiment three by following granularmetric composition, its mass percentage content is :-100～+200 mesh≤5% ,-200～+300 mesh account for 45～50%, remaining is-300 mesh.

2) with the alloy powder of the above-mentioned granularmetric composition of phosphoric acid,diluted solution immersion so that it is powder surface forms dielectric film, add appropriate insulating compound (such as Kaolin or mica powder), lubricant, releasing agent, stir and become compacting powder.

3) being suppressed by above-mentioned powder input dry powder automatic forming press, pressure is 22-24T/cm²Being pressed into annular, compacting specification is external diameter φ 26.90mm, and internal diameter φ 14.70mm, highly 11.20mm, stampings density is 6.8-7.0g/cm³。

4) stampings carry out the protection of heat treatment nitrogen, and temperature is 700-720 DEG C, is incubated 1 hour.

5) detect its magnetic parameter see table:

Claims

1. a manufacture method for iron, silicon, aluminum and nickel alloy powder, including: become fine powder to make annealing treatment with sensing heating, vacuum rapid hardening furnace alloy smelting rapid hardening flakiness shape material Mechanical Crushing broken material heat treatment ball milling, it is characterised in that:

1. the mass percent of alloy component is: Si 4.0～5.0%, Al 3.0～4.0%, Ni1.0～2.5%, Ti 0.1～0.4%, Mn 0.1～0.4%, P 0.1～0.5%, C≤0.02%, remaining for Fe；

2. the raw material used is ingot iron, polysilicon, fine aluminium, pure nickel, titanium sponge and manganese metal, ferrorphosphorus,

Mechanical Crushing granule is 3-10mm, and broken material heat treatment uses hydrogen shield, and temperature is 900-1150 DEG C, temperature retention time 2-4 hour,

Particulate material after described heat treatment, wears into-100 mesh powder with cartridge type ball milling or ring-roller mill, carries out nitrogen protection annealing, and temperature is 800-950 DEG C, is incubated 2-6 hour.