CN102832001B - Iron-base multiphase magnetic alloy material and preparation method thereof - Google Patents

Iron-base multiphase magnetic alloy material and preparation method thereof Download PDF

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CN102832001B
CN102832001B CN201210348728.4A CN201210348728A CN102832001B CN 102832001 B CN102832001 B CN 102832001B CN 201210348728 A CN201210348728 A CN 201210348728A CN 102832001 B CN102832001 B CN 102832001B
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alloy
iron
alloy material
tubular type
type crucible
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CN102832001A (en
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王玲
赵浩峰
刘光宇
林莹莹
郑泽昌
张金花
陆阳平
邱奕婷
张咏
汤朦
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Nanjing University of Information Science and Technology
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Nanjing University of Information Science and Technology
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Abstract

The invention provides an iron-base multiphase magnetic alloy and a preparation method thereof. The alloy not only has low iron loss and high tenacity but also is easy to melt. The preparation method has simple process and low production cost and is suitable for industrial production. The alloy material comprises the following components by weight percent: 3.0-6.0% of Gd, 1.0-3.0% of Si, 1.0-3.0% of Al, 3.0-6.0% of B, 0.05-0.09% of Re, 0.01-0.03% of Tb, 1.0-3.0% of Co and the balance of Fe.

Description

A kind of Iron-base multiphase magnetic alloy material and preparation method thereof
Technical field
The invention belongs to technical field of metal, relate to a kind of iron-based complex phase magnetic alloy and preparation method thereof.
Background technology
No. 200510128543.2 applications provide a kind of Fe base amorphous alloy strip of the excellent in soft magnetic properties under exchanging, it is by there being the pouring nozzle of line of rabbet joint shape peristome to make molten alloy be ejected on the cooling base of movement, make it quench solidification to obtain, the composition of described strip counts more than Fe:78% less than 86% by atom %, more than Si:2% but less than 4%, more than B:2% less than 15%, more than C:0.02% less than 4%, P is represented by symbol M, As, Bi, S, Se, the one kind or two or more of Te is more than M:1% less than 14%, and more than B+M:12% less than 20%, and the iron loss maximum after the annealing at each position of strip Width is designated as Wmax, minimum value is designated as the occasion of Wmin, (Wmax-Wmin)/Wmin is less than 0.4.Strip surface at least side of the noncrystalline parent phase of the P containing 0.2 more than atom % 12 atom below %, has thickness to be the very thin oxide layer of more than 5nm below 20nm.The occasion of impressed frequency 50Hz, maximum externally-applied magnetic field 80A/m AC magnetic field is at Δ T a>=80 DEG C, Δ T bthe peakflux density B obtained under the annealing region of the wide cut of>=60 DEG C 80>=1.35T, B 80standard deviation less than 0.1, iron loss≤0.12W/kg.And, obtain ε fthe resistance to embrittlement characteristic of the excellence of>=0.01.
But the boiling point of the Te in its alloy system is 1390 DEG C, the boiling point of S is 444.674 DEG C, is difficult to operation during fusing.The fusing point of Bi is 271.3 DEG C, and higher than fusing point, metal is easy to oxidation.The iron loss of this alloy also needs to improve in addition.
Summary of the invention
Object of the present invention is exactly for above-mentioned technological deficiency, and provide a kind of iron-based complex phase magnetic alloy, this alloy not only has low iron loss and high tenacity, and alloy melting also easily operates.
Another object of the present invention is to provide a kind of iron-based complex phase magnetic alloy preparation method, and this preparation method's technique is simple, and production cost is low, is suitable for suitability for industrialized production.
The object of the invention is to be achieved through the following technical solutions:
A kind of Iron-base multiphase magnetic alloy material, is characterized in that: in this alloy material, the weight percentage of each composition is: Gd 3.0-6.0%, Si 1.0-3.0%, Al 1.0-3.0%, B 3.0-6.0%, Re 0.05-0.09%, Tb 0.01-0.03%, Co 1.0-3.0%, all the other are Fe.
The tissue characteristic of this iron-based complex phase magnetic alloy be amorphous matrix on be dispersed with part nanometer-size die, the volume of alloy material shared by nanometer-size die is 30-40%.Nanometer-size die is of a size of 80-100nm.
The preparation method of above-mentioned Iron-base multiphase magnetic alloy material, concrete steps are as follows:
(1) first according to the weight percentage of each composition be: Gd 3.0-6.0%, Si1.0-3.0%, Al 1.0-3.0%, B 3.0-6.0%, Re 0.05-0.09%, Tb0.01-0.03%, Co1.0-3.0%, all the other are prepared burden for Fe, and the purity of raw material Si, Al, B, Re, Tb, Co, Fe is all greater than 99.9%, Gd adds in the mode of iron gadolinium intermediate alloy, and in iron gadpolinium alloy, the percentage by weight of Gd is 35%;
(2) raw material is put into vaccum sensitive stove melting, smelting temperature is 1570-1590 DEG C, obtains foundry alloy after cast cooling,
(3) then foundry alloy is put into remelting tubular type crucible and carry out remelting, remelting temperature is 1550-1570 DEG C, described remelting tubular type crucible is placed in vacuum induction forming furnace, the top of remelting tubular type crucible is placed in 2-4mm place under vacuum induction forming furnace runner wheel rim, a fire-resistant plunger moving up and down is placed in remelting tubular type crucible, the gap of this fire-resistant plunger and tubular type crucible inside is 0.5-0.9mm, foundry alloy is placed in the fire-resistant plunger end face fusing in tubular type crucible, with the runner EDGE CONTACT rotated after alloy molten expands and overflows, motlten metal weld pool is pulled formation alloy strip by the circular arc wheel rim on the runner limit that rotates, (fire resisting column moved up and down beyond the Great Wall row time molten alloy liquid is constantly supplied to rotation runner form continuous print alloy strip, )
(4) then alloy strip is placed in 200-300 DEG C, is incubated and within 2-4 hour, obtains the high iron-based of resistance to fragility complex phase magnetic alloy.
In step 4), the linear velocity of vacuum induction forming furnace runner wheel rim is 26 ~ 28m/s, and the thickness of gained alloy strip is 100-300 μm, and width is 3-5 mm.
the present invention has following beneficial effect compared to existing technology:
Tb, Si, B, Gd that alloy material of the present invention adopts can improve amorphous formation ability.Tb, Si, B, Gd in composition exist jointly can make the interphase interaction of cluster Atom strong, then atoms permeating is just difficult, therefore improves material amorphous formation ability.
Al and Co in alloy material provides position for nanocrystalline forming core.Al and Co acting in conjunction, can ensure nanocrystalline formation.
Re, B in alloy material can hinder grain growth.Re, Tb, Si, B combine and can effectively control nanocrystalline formation and grow up.
Re, Al, Gd, Tb in alloy material coordinate can improve grain boundary structure, dissolves local stress, therefore effectively can reduce the fragility of material.
Co in alloy material improves high-temp magnetic performance, the Curie temperature of amorphous increases along with the increase of Co content, and high-temp magnetic conductance also increases with Co content and increases, this is because increase with Co content, nanocrystalline volume fraction increases, and intercrystalline magnetic coupling is strengthened.Al contributes to improving soft magnet performance.Al and Co combines and enhances ferromagnetism effect, effectively improves the magnetic flux of material and reduces the iron loss of material.
Alloy of the present invention, in solidifying, adopts cooling fast and alloying to combine, can effectively reduce the phase size in alloy, ensure being uniformly distributed of chemical composition, both ensure that the magnetic property of alloy, also ensure that the mechanical property of alloy.Heat treatment can reduce the internal stress cooling fast and cause, and improves the toughness of alloy.
In the present invention's preparation, a large amount of use your element rare, institute's cost of material of getting reduces; Alloy is through cooling fast in addition, ensure that the uniformity of alloying component, structure and properties, therefore also just ensure that the quality of alloy.This alloy preparation technology is easy, and process is simple, and the alloy of production has good performance, is very convenient to suitability for industrialized production.Alloy property of the present invention is in table 1.
Accompanying drawing explanation
Fig. 1 is the metallographic structure figure of the material that the embodiment of the present invention 1 obtains.
As can be seen from Fig. 1, the dense structure of iron-based complex phase magnetic alloy of the present invention is even.Volume share shared by this nanocrystal is 30%.
Embodiment
embodiment one:
The preparation method of Iron-base multiphase magnetic alloy material of the present invention, concrete steps are as follows:
(1) first according to the weight percentage of each composition be: Gd 3.0%, Si 1.0%, Al 1.0%, B 3.0%, Re 0.05%, Tb 0.01%, Co 1.0%, all the other are prepared burden for Fe, and the purity of raw material Si, Al, B, Re, Tb, Co, Fe is all greater than 99.9%, Gd adds in the mode of iron gadolinium intermediate alloy, and in iron gadpolinium alloy, the percentage by weight of Gd is 35%;
(2) raw material is put into vaccum sensitive stove melting, smelting temperature is 1580 DEG C, obtains foundry alloy after cast cooling,
(3) then foundry alloy is put into remelting tubular type crucible and carry out remelting, remelting temperature is 1560 DEG C, described remelting tubular type crucible is placed in vacuum induction forming furnace, the top of remelting tubular type crucible is placed in 3mm place under vacuum induction forming furnace runner wheel rim, a fire-resistant plunger moving up and down is placed in remelting tubular type crucible, the gap of this fire-resistant plunger and tubular type crucible inside is 0.6mm, foundry alloy is placed in the fire-resistant plunger end face fusing in tubular type crucible, with the runner EDGE CONTACT rotated after alloy molten expands and overflows, motlten metal weld pool is pulled formation alloy strip by the circular arc wheel rim on the runner limit that rotates, the fire resisting column moved up and down beyond the Great Wall row time molten alloy liquid is constantly supplied to rotation runner form continuous print alloy strip.The linear velocity of vacuum induction forming furnace runner wheel rim is 27m/s, and the thickness of gained alloy strip is 150-250 μm, and width is 3-5mm.
(4) then alloy strip is placed in 250 DEG C, is incubated and within 3 hours, obtains high resistance to fragility Iron-base multiphase magnetic alloy material.Volume share in this alloy material shared by nanocrystal is 30%.
embodiment two:
In Iron-base multiphase magnetic alloy material, the weight percentage of each composition is: Gd 6.0%, Si 3.0%, Al 3.0%, B 6.0%, Re 0.09%, Tb0.03%, Co 3.0%, all the other are Fe.Its preparation process is with embodiment one.Volume share in gained alloy material shared by nanocrystal is 40%.
embodiment three:
In Iron-base multiphase magnetic alloy material, the weight percentage of each composition is: Gd 5.0%, Si 2.0%, Al 2.0%, B 4.0%, Re 0.07%, Tb 0.02%, Co 2.0%, all the other are Fe.Its preparation process is with embodiment one.Volume share in gained alloy material shared by nanocrystal is 35%.
embodiment four: (composition proportion is not within the scope of design proportion of the present invention)
In Iron-base multiphase magnetic alloy material, the weight percentage of each composition is: Gd 2.0%, Si0.5%, Al0.5%, B 2.0%, Re 0.03%, Tb0.005%, Co0.5%, and all the other are Fe.Its preparation process is with embodiment one.Volume share in gained alloy material shared by nanocrystal is 25%.
embodiment five: (composition proportion is not within the scope of design proportion of the present invention)
In Iron-base multiphase magnetic alloy material, the weight percentage of each composition is: Gd 7.0%, Si4.0%, Al 4.0%, B 7.0%, Re 0.1%, Tb 0.04%, Co4.0%, all the other are Fe.Its preparation process is with embodiment one.Volume share in gained alloy material shared by nanocrystal is 50%.
The alloy material one to five of the obtained alloy material of embodiment one to five respectively in corresponding following table, specific performance sees the following form table 1.Peakflux density in following table, for the occasion of magnetic field 80A/m AC magnetic field is at Δ T a>=80 DEG C, Δ T bobtain under the annealing region of the wide cut of>=60 DEG C.
Table 1
Alloy is numbered Alloying component Iron loss/W/kg Peakflux density B 80 /T Resistance to embrittlement characteristic/ε f
Comparative alloy material 200510128543.2 number thin-band material that application is obtained ≤0.12 ≥1.35 ≥0.01
Alloy material one Material prepared by embodiment one 0.11 1.40 0.13
Alloy material two Material prepared by embodiment two 0.09 1.48 0.16
Alloy material three Material prepared by embodiment three 0.10 1.45 0.15
Alloy material four Material prepared by embodiment four 0.13 1.20 0.11
Alloy material five Material prepared by embodiment five 0.12 1.30 0.13
As can be seen from the above table, in material of the present invention, add Fe, Ni, Ho, V, Ru, Al, P, Gd element, contribute to the raising of alloy material soft magnet performance.But content exceeds the scope that the application limits, not only soft magnet performance does not improve, and can reduce on the contrary.Reason is that Gd, Al, Ho, V are too much, and meeting and Co reaction form non-magnetic compound, thus reduce the useful effect of Co.Fe, Ni, Ru element is too much, no longer works, wastes raw material on the contrary, also reduce the useful effect of Co.

Claims (3)

1. an Iron-base multiphase magnetic alloy material, is characterized in that: in this alloy material, the weight percentage of each composition is: Gd 3.0-6.0%, Si 1.0-3.0%, Al 1.0-3.0%, B 3.0-6.0%, Re 0.05-0.09%, Tb 0.01-0.03%, Co 1.0-3.0%, all the other are Fe; The tissue characteristic of this iron-based complex phase magnetic alloy be amorphous matrix on be dispersed with part nanometer-size die, the volume of alloy material shared by nanometer-size die is 30-40%; Nanometer-size die is of a size of 80-100nm.
2. the preparation method of Iron-base multiphase magnetic alloy material described in claim 1, is characterized in that:
(1) first prepare burden according to the above-mentioned weight percentage of each composition, the purity of raw material Si, Al, B, Re, Tb, Co, Fe is all greater than 99.9%, Gd and adds in the mode of iron gadolinium intermediate alloy, and in iron gadpolinium alloy, the percentage by weight of Gd is 35%;
(2) raw material is put into vaccum sensitive stove melting, smelting temperature is 1570-1590 DEG C, obtains foundry alloy after cast cooling,
(3) then foundry alloy is put into remelting tubular type crucible and carry out remelting, remelting temperature is 1550-1570 DEG C, described remelting tubular type crucible is placed in vacuum induction forming furnace, the top of remelting tubular type crucible is placed in 2-4mm place under vacuum induction forming furnace runner wheel rim, a fire-resistant plunger moving up and down is placed in remelting tubular type crucible, the gap of this fire-resistant plunger and tubular type crucible inside is 0.5-0.9mm, foundry alloy is placed in the fire-resistant plunger end face fusing in tubular type crucible, with the runner EDGE CONTACT rotated after alloy molten expands and overflows, motlten metal weld pool is pulled formation alloy strip by the circular arc wheel rim on the runner limit that rotates,
(4) then alloy strip is placed in 200-300 DEG C, is incubated and obtains Iron-base multiphase magnetic alloy material in 2-4 hour.
3. the preparation method of Iron-base multiphase magnetic alloy material according to claim 2, is characterized in that:
In described step 3), the linear velocity of vacuum induction forming furnace runner wheel rim is 26 ~ 28m/s, and the thickness of gained alloy strip is 100-300 μm, and width is 3-5 mm.
CN201210348728.4A 2012-09-19 2012-09-19 Iron-base multiphase magnetic alloy material and preparation method thereof Expired - Fee Related CN102832001B (en)

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US5362339A (en) * 1991-03-14 1994-11-08 Honda Giken Kogyo Kabushiki Kaisha Magnetic refrigerant and process for producing the same
CN101071667A (en) * 2007-04-12 2007-11-14 北京中科三环高技术股份有限公司 Gadolinium-containing Nd-Fe-B rare earth permanent magnetic material dn its manufacturing method
CN101630557A (en) * 2008-07-16 2010-01-20 宁波科宁达工业有限公司 Gadolinium-containing sintered rare earth permanent magnet alloy and preparation method thereof

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JPH10280106A (en) * 1997-04-02 1998-10-20 Minebea Co Ltd Soft magnetic material

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Publication number Priority date Publication date Assignee Title
US5362339A (en) * 1991-03-14 1994-11-08 Honda Giken Kogyo Kabushiki Kaisha Magnetic refrigerant and process for producing the same
CN101071667A (en) * 2007-04-12 2007-11-14 北京中科三环高技术股份有限公司 Gadolinium-containing Nd-Fe-B rare earth permanent magnetic material dn its manufacturing method
CN101630557A (en) * 2008-07-16 2010-01-20 宁波科宁达工业有限公司 Gadolinium-containing sintered rare earth permanent magnet alloy and preparation method thereof

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