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CN100519013C - Fe-Ni50 series alloy powder and magnetic powder core manufacturing method - Google Patents

Fe-Ni50 series alloy powder and magnetic powder core manufacturing method Download PDF

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CN100519013C
CN100519013C CNB2006100181604A CN200610018160A CN100519013C CN 100519013 C CN100519013 C CN 100519013C CN B2006100181604 A CNB2006100181604 A CN B2006100181604A CN 200610018160 A CN200610018160 A CN 200610018160A CN 100519013 C CN100519013 C CN 100519013C
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magnetic
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heat treatment
alloy powder
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CN100999021A (en
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王茜
王�锋
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WUHAN XINDA MAGNETISM MATERIAL CO Ltd
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Abstract

The present invention relates to a preparation method of soft magnetic Fe-Ni50 system alloy powder. Said method includes the following steps: smelting Fe-Ni50 system alloy, spraying to obtain powder by adopting water atomization process, processing said powder, making heat treatment, passivation treatment, adding insulating agent, lubricating agent and demoulding agent into the alloy powder, mould-pressing and forming, heat treatment and coating surface.

Description

Fe-Ni 50Series alloy powder and magnetic core, manufacturing method
Technical field
The present invention relates to the manufacturing technology field of magnetic bodies, specifically a kind of Fe-Ni 50Series alloy powder and magnetic core, manufacturing method.
Background technology
In recent years, the high speed development of electron electric power industry requires the energy-conservation of electronic equipment, instrument, and electronic unit is followed in miniaturization, the high efficiency of components and parts, miniaturization.In frequency is 10kH z-500kH zNow widely apply ferrocart core in the scope, but power attenuation is bigger, Effective permeability about 75.Fe-Ni 50Be alloy magnetic powder core, also claim high flux magnetic core, it has the saturation flux density height, core loss is little, and the magnetic device iron core that is used as high frequency, high-power, high D.C. magnetic biasing or the close peak value of high AC magnetism has advantage.Fe-Ni in the magnetic core 50The saturation magnetic induction of magnetic core is maximum about 1.5T (tesla), D.C. magnetic biasing ability height.
The Japan Patent spy opens 2000-173817 and adopts Ni35-55%, and surplus is the composition of Fe, and aerosolization method metal dust length-width ratio is 1~5, surface oxidation thickness 0.01~0.05 μ m, can form the high-quality compressed-core alloy powder of high pack completeness, example average grain diameter 80 μ m, 10t/cm 2Pressure, Ar gas shiled heat treatment in 650 ℃ * 30 minutes, the result shows that loss is lower, but magnetic conductivity μ e=86~97 are lower than commercial μ e=125, does not also point out to hand over the drop performance after the straight stack.
The Japan Patent spy opens 2000-239702 and adopts Ni:35~85%, Si:1.0~4.5% and below the Mn:0.15%, and Si/Mn〉20, in addition below the AL:0.5%, below the Mo:5.5%, surplusly be the Fe composition, water spray powder and require crystallization particle diameter d/D 500.10 wherein d be the average crystallite particle diameter, D 50Be average grain diameter.Example 1 is pointed out Ni46.8-47.3%, Si/Mn21.7-42.1, and its μ e=102~120, loss 19.9~37.1W/Kg is d/D wherein 500.10 requirement is difficult realizes that magnetic conductivity is yet on the low side.
The Japan Patent spy opens 2001-23811 and adopts Ni45-68%, and interpolation IVB family elements Si, Ge, Sn are 0.1~6.5wt%, smelt back usefulness gas and add water atomization powder process, example 3Ni50.2% wherein, Si1.1%, Ge3.8%, surplus is the Fe composition, its μ e=87, loss 100kH z1000G S, P=98bkw/m 3, magnetic conductivity is more on the low side than commercial μ e125.
In the recent period the Japan Patent spy to open 2005-82853 be that the Fe-Ni of Fe-50wt% is that non-retentive alloy adds each 0.4Nt% of Cr, Mn/following total amount and is no more than 0.8wt%, water atomization powder process generates spherical, and loss is low, interior resistance height, adopt vacuum metling, loss 243-284kw/m 3, do not indicate magnetic conductivity and alternating current-direct current stack performance.Estimate that its magnetic conductivity only is μ e~60.
Summary of the invention
The objective of the invention is to design a kind of soft-magnetic Fe-Ni that overcomes 50Existing above-mentioned technological deficiency in the manufacture method of series alloy powder and magnetic core provides a kind of technology comparatively convenient, and the powder core magnetic conductivity of producing is that 125 alternating current-direct currents stack back magnetic descends slowly the new manufacture method that power attenuation is low.
A kind of soft-magnetic Fe-Ni of the present invention 50The series alloy powder manufacture method comprises the steps: Fe-Ni 50Smelting-the water atomization that is alloy is sprayed into powder-powder processing-powder heat treatment, it is characterized in that:
A: the composition of alloy is a nickel 49~50%, manganese 0.1~0.6%, titanium 0.1~0.6%, and Mn+Ti 〉=0.6%, and Yu Weitie selects for use the nitrogen protection induction furnace to smelt;
B: the method atomisation of the molten steel water spray after the refining, water-cooled becomes approximate globular powder, and particle diameter is-100 orders;
C: will be similar to globular powder with Mechanical Method and be processed into sheet, and be preferably flat;
D: flakelike powder is heated 800 ± 20 ℃ under the pure hydrogen protection, be incubated 2-4 hour.
Compare with other milling methods; the present invention has following technical characterstic: adding Mn and Ti can crystal grain thinning; improve resistivity in the alloy; power attenuation to reduction magnetic core is useful; smelt than common smelting with nitrogen protection; oxygen content can reduce in its alloy; it is more cheap and feasible that atomization dusts; powder is processed into the compressibility that sheet can be improved compression molding; improve the pack completeness of powder, pure hydrogen protection heat treatment is to eliminate stress and reduce oxygen content, nitrogen content and removal impurity in the alloyed powder.
A kind of Fe-Ni of the present invention 50Be the manufacture method of alloy soft magnetic powder core, comprise the steps: to sieve the powder particle granularity and carry out grain size proportion-powder surface Passivation Treatment-in alloy powder, add insulating compound, bonding agent, releasing agent-compression molding-heat treatment-face coat.
Compare with other manufacture methods, the present invention has following technical characterstic: grain size proportion is to be undertaken by the magnetic conductivity of the magnetic core of making, for example: μ e=125,-100 orders /+200 orders are about 10%,-200 orders /+300 orders are about 60%, surplus is-300 orders, if make the magnetic core of μ e=60, then needs all to adopt-300 powder materials.The powder surface Passivation Treatment is to make powder surface generate a kind of oxide-film; its thickness is about 0.1 μ m; increase resistivity; add insulating compound; bonding agent; releasing agent then is the requirement of compression molding; should reach certain density; do not produce pressure check again and be easy to the demoulding; compression molding is to make its moulding product complete by certain pressure, reaches certain magnetic property, and heat treatment is to carry out under nitrogen protection; make the manufactured goods unlikely oxidation in surface; the process that the while magnetic property improves greatly, face coat is the requirement that iron inductance is made in next procedure, the insulating properties of its coating is that dielectric medium intensity reaches in 1000V.
The specific embodiment
Embodiment one:
With ingot iron; the nickel plate; manganese metal; titanium sponge drops into interior smelting of induction furnace of nitrogen protection; smelting into chemical composition is nickel 49~50%; manganese 0.1~0.6%; titanium 0.1~0.6%; and Mn+Ti 〉=0.6%; the alloy molten steel of Yu Weitie, water water spray cold process is sprayed molten steel become-100 purpose powder, and powder for drying is about 100 ℃; be processed into sheet with Mechanical Method; enter heat-treatment furnace, under hydrogen shield, 800 ℃ ± 20 ℃ reduction were handled 2-4 hour; after the cooling with its screening; account for 10 ± 5% according to the 100-200 order, the 200-320 order accounts for 50 ± 5%, and is surplus for less than 320 purpose fine powders the alloy powder granularity is allocated; carry out the powder surface Passivation Treatment with acid solution afterwards; surface at alloy powder forms coating film, insulate with thin mica powder or kaolin, and consumption is 0.2~1.0%; make bonding agent with sodium silicate solution; add releasing agent after above-mentioned powder stirred, fry and do or oven dry, promptly can be used as the compacting powder.This powder is dropped in ¢ 26.90/ ¢ 14.70 ring moulds, with 14~18T/cm 2Pressure to be pressed into height be 11.2 millimeters, heat-treat after the compression moulding, 700 ℃ of insulations are 1.5 hours under nitrogen protection, the cooling back was carried out stabilization processes in 3 hours 200 ℃ of insulations.Example chemical composition: Ni:49.0%, Mn:0.2%, Ti:0.6%, surplus is Fe.Its magnetic property basic parameter such as table 1:
Figure C200610018160D00071
Table 1 data show, the inductance factors A of sample 1 L=157 (1 ± 8%) nH/N 2Scope in, corresponding Effective permeability (μ e) is 125, the magnetic conductivity that exchanges after the stack descends 18%, its loss is less, is higher than the magnetic property that existing method is made.
Embodiment two: process is with example one, and its alloying component is: Ni:49.6%, and Mn:0.5%, Ti:0.2%, surplus is Fe.Its magnetic property basic parameter such as table 2:
Table 2 data show, compare with embodiment one, and Mn, some variation of Ti content, the magnetic conductivity that exchanges after superposeing descends variation not quite, and its loss has increase slightly, but lower than commercial product.
Embodiment three:
Process is with example one, and its alloying component is: Ni:49.8%, and Mn:0.4%, Ti:0.6%, surplus is Fe.Its magnetic property basic parameter such as table 3:
Figure C200610018160D00081
Table 3 data show, compare with embodiment one, and Mn, Ti content all increase to some extent, and the magnetic conductivity decline that exchanges after superposeing is fast slightly, μ e=81% μ 0Its loss has decline slightly, and this may be the crystal grain effect of refinement generation more.
Embodiment four:
Process is with example one, and its alloying component is: Ni:49.8%, and Mn:0.3%, Ti:0.5%, surplus is Fe.Flakelike powder is through hydrogen shield heat treatment, and its temperature is 800 ℃ of insulations after 2.5 hours, and recording the powder oxygen content is 150ppm, its magnetic property basic parameter such as table 4:
Figure C200610018160D00082
Table 4 data show that after powder was processed into sheet, heat of reduction was handled under hydrogen shield, and lower 800 ℃ of following 2.5 hours its oxygen content, magnetic property is also more satisfactory.If 850 ℃ of following heat treatments, powder easily bonds, and also needing increases residual stress with its processing refinement, and its coercivity is increased, and reduces magnetic conductivity.
Need to prove; in the above-described embodiments; heat treatment after the compression moulding is the following 700 ℃ of insulations of nitrogen protection 1.5 hours; be to be example with sample specification ¢ 26.90/ ¢ 14.70 * 11.20 (be that external diameter is 26.90mm, internal diameter is 14.70mm, highly is 11.20mm); if sample size is little; its volume is little, but the heat treatment temperature retention time tip is short, but must be greater than 30 minutes.

Claims (1)

1, a kind of soft-magnetic Fe-Ni 50The series alloy powder manufacture method comprises: Fe-Ni 50Be the heat treatment after the smelting-water atomization of alloy is sprayed into powder-powder processing-processing, it is characterized in that:
A: the composition of alloy is a nickel 49~50%, manganese 0.1~0.6%, titanium 0.1~0.6%, and Mn+Ti 〉=0.6%, and Yu Weitie selects for use the nitrogen protection induction furnace to smelt;
B: water water spray cold being atomized into-100 purpose powder;
C: the powder of water atomization is processed into sheet;
D: flakelike powder is through hydrogen shield heat treatment, and its temperature is: 800 ± 20 ℃, and 2-4 hour.
CNB2006100181604A 2006-01-13 2006-01-13 Fe-Ni50 series alloy powder and magnetic powder core manufacturing method Expired - Fee Related CN100519013C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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TWI682040B (en) * 2018-01-17 2020-01-11 日商同和電子科技有限公司 Fe-Ni ALLOY POWDER AND COMPACT FOR INDUCTOR AND INDUCTOR USING THE SAME

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CN102436894B (en) * 2011-12-27 2014-08-20 浙江大学 Preparation method of high-frequency high-magnetic-permeability low-loss iron nickel molybdenum metal magnetic powder core
CN103172359B (en) * 2013-03-25 2014-05-07 海宁联丰磁业股份有限公司 Manganese zinc power ferrite magnetic powder core and preparation method thereof
CN103600069A (en) * 2013-12-02 2014-02-26 北矿磁材科技股份有限公司 Magnetic flaky metal powder surface treating method
CN103752837A (en) * 2013-12-12 2014-04-30 金川集团股份有限公司 Method for producing water atomized alloy powder by using reduced iron of smelting slag
JP6345146B2 (en) * 2015-03-31 2018-06-20 太陽誘電株式会社 Coil parts
CN106252013B (en) * 2016-08-19 2018-08-17 横店集团东磁股份有限公司 A kind of preparation method of the iron of μ=60 nickel soft-magnetic powder core
CN109273233A (en) * 2018-09-19 2019-01-25 上海岱梭动力科技有限公司 The preparation method and magnetic core of magnetic core
CN111477442A (en) * 2019-01-24 2020-07-31 昆山玛冀电子有限公司 Method for improving cracking phenomenon of molded inductor after baking
CN110957123A (en) * 2019-12-17 2020-04-03 山西中磁尚善科技有限公司 Method for preparing iron-nickel soft magnetic powder core with magnetic conductivity of 125
CN113528984A (en) * 2021-01-15 2021-10-22 武汉科技大学 FeSiPC amorphous soft magnetic alloy and preparation method thereof
CN114951668A (en) * 2022-05-31 2022-08-30 清远市晶瑞合金材料有限公司 Soft magnetic powder for 3D printing and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI682040B (en) * 2018-01-17 2020-01-11 日商同和電子科技有限公司 Fe-Ni ALLOY POWDER AND COMPACT FOR INDUCTOR AND INDUCTOR USING THE SAME

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