CN104498806A - Preparation method of iron-cobalt-based soft magnetic material - Google Patents
Preparation method of iron-cobalt-based soft magnetic material Download PDFInfo
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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
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- iron
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- 239000000696 magnetic material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- QVYYOKWPCQYKEY-UHFFFAOYSA-N [Fe].[Co] Chemical compound [Fe].[Co] QVYYOKWPCQYKEY-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 239000000956 alloy Substances 0.000 claims abstract description 43
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052742 iron Inorganic materials 0.000 claims abstract description 11
- 239000011241 protective layer Substances 0.000 claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 5
- 238000004381 surface treatment Methods 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 8
- 238000010891 electric arc Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000007669 thermal treatment Methods 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005275 alloying Methods 0.000 claims description 4
- JPUHCPXFQIXLMW-UHFFFAOYSA-N aluminium triethoxide Chemical compound CCO[Al](OCC)OCC JPUHCPXFQIXLMW-UHFFFAOYSA-N 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 239000000470 constituent Substances 0.000 claims description 4
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 abstract description 11
- 230000005291 magnetic effect Effects 0.000 abstract description 10
- 230000007797 corrosion Effects 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 8
- 230000035699 permeability Effects 0.000 abstract description 5
- 229910017052 cobalt Inorganic materials 0.000 abstract description 4
- 239000010941 cobalt Substances 0.000 abstract description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract 1
- 229910052777 Praseodymium Inorganic materials 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 1
- 229910052796 boron Inorganic materials 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000005292 diamagnetic effect Effects 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000005300 metallic glass Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910000889 permalloy Inorganic materials 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- -1 silicon praseodymium boron Chemical compound 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Landscapes
- Soft Magnetic Materials (AREA)
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
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.
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Cited By (2)
| 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 |
-
2015
- 2015-01-17 CN CN201510022773.4A patent/CN104498806A/en active Pending
Cited By (2)
| 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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