CN104498806A - Preparation method of iron-cobalt-based soft magnetic material - Google Patents

Preparation method of iron-cobalt-based soft magnetic material Download PDF

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CN104498806A
CN104498806A CN201510022773.4A CN201510022773A CN104498806A CN 104498806 A CN104498806 A CN 104498806A CN 201510022773 A CN201510022773 A CN 201510022773A CN 104498806 A CN104498806 A CN 104498806A
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soft magnetic
alloy
magnetic materials
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iron
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王中克
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Xia Keche
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Abstract

The invention relates to a preparation method of an iron-cobalt-based soft magnetic material. A main soft magnetic material body is made of an alloy material in the atom ratio as follows: Fe(100-a-b-c-d-e-f)CoaSibCrcPrdBeTif, wherein the a ranges from 27 to 35, the b ranges from 2 to 3, the c ranges from 3 to 5, the d ranges from 1 to 2, the e ranges from 5 to 6, and the f ranges from 4 to 6. The preparation method comprises the following steps that (1) a main alloy body is prepared, (2) the main soft magnetic material body is prepared, and (3) surface treatment is conducted. According to the soft magnetic material prepared through the preparation method, iron and cobalt are used as main materials so as to obtain high magnetic permeability; the silicon element, the praseodymium element and the boron element are appropriately added so as to improve the magnetic saturation resistance capacity of the material; the Cr and the Ti are added to the material, and an aluminum oxide protective layer is formed in the soft magnetic material so as to improve corrosion resistance performance of the material.

Description

A kind of preparation method of iron cobalt-based soft magnetic materials
Technical field
The present invention relates to a kind of preparation method of iron cobalt-based soft magnetic materials.
Background technology
Fe-based amorphous and nanometer crystal alloy is widely used in the fields such as microelectronics, machinery, power engineering owing to having excellent soft magnetic performance, corrosion resistance nature etc.
The outstanding advantages of this type of alloy is the high magnetic strength and the high magnetic permeability of cobalt base amorphous alloy, the low iron loss that have had both Fe-based amorphous alloy, therefore cobalt base amorphous alloy, crystalline state permalloy and ferrite can be replaced, in high-frequency power electronic and electronic information field, there is wide application prospect, the object reducing volume, reduce costs can be reached.
But as everyone knows, the amorphous formation ability of alloy and solidity to corrosion are all quite responsive to its composition.Normal conditions are, in order to obtain the iron-base large-block amorphous alloy of high anti-corrosion, must add a large amount of non-ferromagnetic elements, and this, by causing the reduction of this alloy saturation induction density and Curie temperature, even loses ferromegnetism under room temperature.Therefore, develop the iron-based soft magnetic non-crystaline amorphous metal simultaneously with high anti-corrosion, high saturated magnetic induction and high amorphous formation ability and be still the difficult problem needing to be captured so far.
Summary of the invention
The invention provides a kind of preparation method of iron cobalt-based soft magnetic materials, cobalt-based magnetic core prepared by the method has high magnetic permeability, high resistance magneticsaturation high-corrosion resistance.
To achieve these goals, the invention provides a kind of preparation method of iron cobalt-based soft magnetic materials, wherein this soft magnetic materials main body uses the alloy material of following atom ratio to make: Fe (100-a-b-c-d-e-f)co asi bcr cpr db eti f, wherein: a=27-35, b=2-3, c=3-5, d=1-2, e=5-6, f=4-6, the method comprises the steps:
(1) bulk alloy is prepared
Purity is greater than raw material Fe, Co, Si, Cr, Pr, B and Ti of 99.9%, by Fe (100-a-b-c-d-e)co asi bcr cpr db eti falloying constituent weighs with atomic percent and prepares burden, and dysprosium adds in the mode of iron disprosium alloy; Electric arc furnace is evacuated to vacuum tightness 1-2 × 10 -5pa, then counter fill purity be the Ar gas of 99.999% to 1-2 normal atmosphere, add above-mentioned raw materials, open more than electric arc furnace heating alloys fusing point, then change different directions melting 4-5 time repeatedly, injection mold cools down is master alloy ingot, formation mother alloy;
(2) soft magnetic materials main body is prepared
Mother alloy is removed surface scale, and after hydrogen is broken, ball milling becomes particle diameter to be the powdered alloy of 10-15 μm, powdered alloy is molded into the soft magnetic materials main body green compact of predetermined shape;
After above-mentioned soft magnetic materials main body green compact are put into vacuum high-temperature resistance furnace, be warming up to 1250-1350 DEG C with the heat-up rate of 10-15 DEG C/min, after insulation 2-3h, with the cooling rate isothermal annealing of 5-10 DEG C/min to room temperature, obtain soft magnetic materials main body;
(3) surface treatment
Be dissolved in ethylene glycol solvent by by aluminum ethylate; forming concentration is the solution of 5-10wt%; above-mentioned soft magnetic materials main body is immersed 10-15min in described solution; after taking-up, in air atmosphere, thermal treatment 1-2h; thermal treatment temp is 650-700 DEG C; form fine and close protective layer of alumina, after naturally cooling, obtain product.
Soft magnetic materials prepared by the present invention; iron cobalt is adopted to be that material of main part is to obtain high permeability; suitable interpolation silicon praseodymium boron, to improve the diamagnetic saturability of material, adds Cr and Ti in the material and forms protective layer of alumina to improve the corrosion resistant performance of material at soft magnetic materials.
Embodiment
embodiment one
The soft magnetic materials of the present embodiment uses the alloy material of following atom ratio to make: Fe 58co 27si 2cr 3pr 1b 5ti 4.
Purity is greater than raw material Fe, Co, Si, Cr, Pr, B and Ti of 99.9%, by Fe 58co 27si 2cr 3pr 1b 5ti 4alloying constituent weighs with atomic percent and prepares burden, and dysprosium adds in the mode of iron disprosium alloy; Electric arc furnace is evacuated to vacuum tightness 1 × 10 -5pa, then instead fills Ar gas to 1 normal atmosphere that purity is 99.999%, adds above-mentioned raw materials, opens more than electric arc furnace heating alloys fusing point, and then change different directions melting 4 times repeatedly, injections mold cools down is master alloy ingot, formation mother alloy.
Mother alloy is removed surface scale, and after hydrogen is broken, ball milling becomes particle diameter to be the powdered alloy of 10-15 μm, powdered alloy is molded into the soft magnetic materials main body green compact of predetermined shape.
After above-mentioned soft magnetic materials main body green compact are put into vacuum high-temperature resistance furnace, be warming up to 1250 DEG C with the heat-up rate of 10 DEG C/min, after insulation 3h, with the cooling rate isothermal annealing of 5 DEG C/min to room temperature, obtain soft magnetic materials main body.
Be dissolved in ethylene glycol solvent by by aluminum ethylate, forming concentration is the solution of 5wt%, and above-mentioned soft magnetic materials main body is immersed 15min in described solution, after taking-up; in air atmosphere, thermal treatment 2h, thermal treatment temp is 650 DEG C; form fine and close protective layer of alumina, after naturally cooling, obtain product.
embodiment two
The soft magnetic materials of the present embodiment uses the alloy material of following atom ratio to make: Fe 43co 35si 3cr 5pr 2b 6ti 6.
Purity is greater than raw material Fe, Co, Si, Cr, Pr, B and Ti of 99.9%, by Fe 43co 35si 3cr 5pr 2b 6ti 6alloying constituent weighs with atomic percent and prepares burden, and dysprosium adds in the mode of iron disprosium alloy; Electric arc furnace is evacuated to vacuum tightness 2 × 10 -5pa, then instead fills Ar gas to 2 normal atmosphere that purity is 99.999%, adds above-mentioned raw materials, opens more than electric arc furnace heating alloys fusing point, and then change different directions melting 5 times repeatedly, injections mold cools down is master alloy ingot, formation mother alloy.
Mother alloy is removed surface scale, and after hydrogen is broken, ball milling becomes particle diameter to be the powdered alloy of 10-15 μm, powdered alloy is molded into the soft magnetic materials main body green compact of predetermined shape.
After above-mentioned soft magnetic materials main body green compact are put into vacuum high-temperature resistance furnace, be warming up to 1350 DEG C with the heat-up rate of 15 DEG C/min, after insulation 2h, with the cooling rate isothermal annealing of 10 DEG C/min to room temperature, obtain soft magnetic materials main body.
Be dissolved in ethylene glycol solvent by by aluminum ethylate, forming concentration is the solution of 10wt%, and above-mentioned soft magnetic materials main body is immersed 10min in described solution, after taking-up; in air atmosphere, thermal treatment 1h, thermal treatment temp is 700 DEG C; form fine and close protective layer of alumina, after naturally cooling, obtain product.
comparative example
According to chemical composition Fe 39co 45al 4mo 1zr 6b 4cu 1proportioning takes raw metal, puts into arc-melting furnace, melting 3 times.After mother alloy fragmentation, put into single roller and revolve stove of quenching and revolve and quench, nozzle is 0.5mm to the spacing of copper roller, and the linear velocity of copper roller is 30m/s, and spray pressure is 0.5Mpa, obtains amorphous nano peritectic alloy, and its thickness is 25 μm, and width is 5mm.Alloy strip winding is cut into the soft magnetic materials of predetermined size and shape.
Carry out magnetic property to the soft magnetic materials of the embodiment 1-2 and comparative example with same shape and size and test its corrosion resistance nature in the sour environment of humidity, the Ph value of the sour environment of described humidity is 5.5.Test result shows: the permeability of the soft magnetic materials that embodiment 1-2 obtains and the soft magnetic materials of diamagnetic saturation intensity comparative example improve more than 10 and 15% respectively, and corrosion resistance improves more than 2 times (corrosion resistance is in the inverses of corrosion speed).

Claims (1)

1. a preparation method for iron cobalt-based soft magnetic materials, wherein this soft magnetic materials main body uses the alloy material of following atom ratio to make: Fe (100-a-b-c-d-e-f)co asi bcr cpr db eti f, wherein: a=27-35, b=2-3, c=3-5, d=1-2, e=5-6, f=4-6, the method comprises the steps:
(1) bulk alloy is prepared
Purity is greater than raw material Fe, Co, Si, Cr, Pr, B and Ti of 99.9%, by Fe (100-a-b-c-d-e)co asi bcr cpr db eti falloying constituent weighs with atomic percent and prepares burden, and dysprosium adds in the mode of iron disprosium alloy; Electric arc furnace is evacuated to vacuum tightness 1-2 × 10 -5pa, then counter fill purity be the Ar gas of 99.999% to 1-2 normal atmosphere, add above-mentioned raw materials, open more than electric arc furnace heating alloys fusing point, then change different directions melting 4-5 time repeatedly, injection mold cools down is master alloy ingot, formation mother alloy;
(2) soft magnetic materials main body is prepared
Mother alloy is removed surface scale, and after hydrogen is broken, ball milling becomes particle diameter to be the powdered alloy of 10-15 μm, powdered alloy is molded into the soft magnetic materials main body green compact of predetermined shape;
After above-mentioned soft magnetic materials main body green compact are put into vacuum high-temperature resistance furnace, be warming up to 1250-1350 DEG C with the heat-up rate of 10-15 DEG C/min, after insulation 2-3h, with the cooling rate isothermal annealing of 5-10 DEG C/min to room temperature, obtain soft magnetic materials main body;
(3) surface treatment
Be dissolved in ethylene glycol solvent by by aluminum ethylate; forming concentration is the solution of 5-10wt%; above-mentioned soft magnetic materials main body is immersed 10-15min in described solution; after taking-up, in air atmosphere, thermal treatment 1-2h; thermal treatment temp is 650-700 DEG C; form fine and close protective layer of alumina, after naturally cooling, obtain product.
CN201510022773.4A 2015-01-17 2015-01-17 Preparation method of iron-cobalt-based soft magnetic material Pending CN104498806A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107893199A (en) * 2017-11-23 2018-04-10 海盐中达金属电子材料有限公司 A kind of Co27 siderochrome cobalt magnetically soft alloy steel band
US20210313110A1 (en) * 2020-04-02 2021-10-07 Seiko Epson Corporation Method For Manufacturing Dust Core And Dust Core

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107893199A (en) * 2017-11-23 2018-04-10 海盐中达金属电子材料有限公司 A kind of Co27 siderochrome cobalt magnetically soft alloy steel band
US20210313110A1 (en) * 2020-04-02 2021-10-07 Seiko Epson Corporation Method For Manufacturing Dust Core And Dust Core

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