CN102709018A - Iron-based ternary nanocrystalline magnetically soft alloy with low cost and high soft magnetism property as well as preparation method thereof - Google Patents
Iron-based ternary nanocrystalline magnetically soft alloy with low cost and high soft magnetism property as well as preparation method thereof Download PDFInfo
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- CN102709018A CN102709018A CN2012101611959A CN201210161195A CN102709018A CN 102709018 A CN102709018 A CN 102709018A CN 2012101611959 A CN2012101611959 A CN 2012101611959A CN 201210161195 A CN201210161195 A CN 201210161195A CN 102709018 A CN102709018 A CN 102709018A
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Abstract
The invention provides an iron-based ternary nanocrystalline magnetically soft alloy with low cost and high soft magnetism property as well as a preparation method of the iron-based ternary nanocrystalline magnetically soft alloy, belonging to the field of preparation of a magnetic soft alloy in a functional material. The nanocrystalline magnetically soft alloy is characterized in that a chemical composition of the nanocrystalline magnetically soft alloy can be represented as FeaPbCuc, wherein a, b and c are atomic percentages of corresponding component, and has a variation range as follows: b is equal to 14-19, c is equal to 0.5-1.5, and a is equal to (100-b-c). The preparation method comprises the steps of: at first, preparing according to the requirements of the components of the alloy provided by the invention, and obtaining a mother alloy with the uniform components; secondly, heating the mother alloy to be fused, and rapidly cooling the mother alloy by injecting on a copper roller through a nozzle so as to prepare an amorphous thin belt; and finally, crystallizing and annealing the amorphous thin belt obtained by rapid quenching at a certain temperature so as to obtain the nanocrystalline magnetically soft alloy. The iron-based ternary nanocrystalline magnetically soft alloy provided by the invention has the advantages of few elements, low cost and high soft magnetism property, and can be widely applied to the field of an electric transformer, a mutual inductor and the like by replacing the conventional silicon steel sheet and the conventional iron-based amorphous nanocrystalline magnetically soft alloy.
Description
Technical field
The invention belongs to the technical field of magnetically soft alloy in the functional material, relate to iron-based ternary nanocrystals magnetically soft alloy of a kind of low cost, high soft magnet performance and preparation method thereof specifically.
Background technology
The Yoshizawa of Hitachi, Ltd in 1988 has developed the FINEMET alloy, its typical composition Fe
73.5Si
13.5B
9Cu
1Nb
3, in view of its excellent soft magnet performance, nano-crystal soft magnetic alloy has caused the very big interest of academia and industrial quarters.Though iron-base nanometer crystal alloy is compared saturation induction density not as good as the latter with soft magnetism silicon steel commonly used at present, its loss is 1/3 ~ 1/5 of a silicon steel under the same terms, particularly is used on the distribution transformer and can reduces no-load loss greatly.Iron-base nanometer crystal alloy is compared with soft magnetic ferrite, when being lower than 50kHz, has the work magnetic strength that is higher than 2 ~ 3 times of soft magnetic ferrites on more low-loss basis having, and core volume can be little more than 1 times.Recent study person constantly develops the nano-crystal soft magnetic alloy system that makes new advances; The more representative Fe-M-B-Cu as having high saturated magnetic induction is (M=Zr, Hf, Nb etc.) NANOPERM alloy, has (Fe-Co)-M-B-Cu system (M=Zr, Hf, Nb etc.) HITPERM alloy of high-temperature stability.Fe-based nanocrystalline magnetically soft alloy is widely used in every field at present, like fields such as high frequency transformer, high-frequency converter, current transformer, earth leakage circuit-breaker, common mode inductance iron cores.
Yet, traditional Fe-based amorphously often add a certain proportion of Co and replace Fe in order to improve saturation induction density, Bs can be up to 1.8T [document sees reference: J.A.Vaccari, Des. Eng. 52 (1981) 53].To obtain being uniformly distributed in the nano-crystal soft magnetic alloy of matrix easily in order annealing, often to add preceding transiting group metal elements such as a certain amount of Nb, Zr, Mo again, like the 1K107 (Fe-Si-B-Cu-Nb series) that now is widely used in production practices now.And in order to improve amorphous formation ability, the researcher often adds a certain amount of B element [document sees reference: Thin Solid Films 519 (2011) 8283 – 8286] both at home and abroad.Noble element Nb, Zr, being added in of B have increased cost of material greatly when improving its performance, therefore limited its large-scale promotion application to a certain extent.And in order to obtain high-quality amorphous precursor body; Present technical recipe often contains two or more vitrifying element; Increasing of element kind not only increased the difficulty of preparing burden in actual production process; Homogeneity of ingredients also is difficult to control in fusion process simultaneously, can only so not only increase energy consumption and also reduce efficient through increasing smelting time and melting number of times.
Summary of the invention
The object of the present invention is to provide that a kind of constituent element is few, low-cost, the iron-based ternary nanocrystals magnetically soft alloy of high soft magnet performance and preparation method thereof.
The present invention realizes through following technical scheme:
The iron-based ternary nanocrystals magnetically soft alloy of a kind of low cost, high soft magnet performance, it is characterized in that: the chemical composition of this nano-crystal soft magnetic alloy can be expressed as Fe
aP
bCu
c, wherein a, b, c represent respectively the atomic percentage of corresponding component, excursion: b=14 ~ 19, c=0.5 ~ 1.5, a=1-b-c.
The iron-based ternary nanocrystals magnetically soft alloy of low cost of the present invention, high soft magnet performance, its characteristic component is: Fe
80P
19Cu
1Or Fe
83P
16.5Cu
0.5Or Fe
84.5P
14Cu
1.5
The preparation method of the iron-based ternary nanocrystals magnetically soft alloy of low cost of the present invention, high soft magnet performance comprises following process:
Step 1, prepare burden and the foundry alloy that is evenly distributed of smelting component according to alloying component;
Why Fe-based nanocrystalline magnetically soft alloy of the present invention only contains a kind of vitrifying element P, and does not contain B and other vitrifying element just can successfully obtain the amorphous precursor body.Choosing of alloying component of the present invention made full use of the Fe-P-Cu ternary alloy phase diagram between near the Composition Region the eutectic point because near the amorphous formation ability of alloy eutectic point often the amorphous formation ability than other composition points is strong.Can know that by thermodynamics the enthalpy of mixing △ H of Fe and Cu is positive (13kJ/mol), the enthalpy of mixing △ H of P and Cu is (9kJ/mol), this means between Fe and the Cu to exist repulsion, exist gravitation between P and the Cu of bearing.The microcell that in revolving the process of quenching, is rich in P and Cu so forms in matrix, the higher potential core that forms nanocrystalline α-Fe when annealing that becomes of Fe content around these microcells.Such amorphous precursor object constructional features just easily at lower temperature, obtains having the amorphous/nanocrystalline fresh surfaces of excellent soft magnet performance than other amorphous soft-magnetic alloy under the annealing conditions of short period annealing.
Fe-based nanocrystalline magnetically soft alloy of the present invention does not contain elements such as valuable Co, Zr, Nb, B; With low cost, constituent element is few, and the melting uniformity is controlled easily in the production process; The annealing temperature of the more present most amorphous bands of amorphous band of this composition system is low simultaneously; Temperature retention time is short, and not only production efficiency is high in process of production, and the energy consumption of specific yield reduces greatly.And take the technology with the stove cooling after the annealing of this laboratory sample, do not adopt the general beforehand research test insulation back technology of cooling fast, this annealing process is more near production practices.Final result shows: under suitable subsequent annealing process conditions, and the saturation induction density B of this alloying component system
sCan reach 1.75T, coercive force H
cMinimumly 3.5A/m can be reached, the iron based nano crystal band of excellent soft magnet performance can be obtained to have.Therefore, alloy of the present invention is more suitable for large-scale production, and existing silicon steel sheet of instead and Fe-based amorphous, nano-crystal soft magnetic alloy are applied to fields such as electric power electric transformer, instrument transformer.
Description of drawings
Accompanying drawing 1 is the embodiment of the invention 1,2, and 3 is Fe
80P
19Cu
1Fe
83P
16.5Cu
0.5Fe
84.5P
14Cu
1.5The magnetic hysteresis loop of nano-crystal soft magnetic alloy.Ordinate is magnetic induction density B (T), and abscissa is magnetic field intensity H (kA/m).For the coercivity H of the example that clearly draws each enforcement, the illustration of accompanying drawing 1 has provided near the magnetic hysteresis loop enlarged drawing of each embodiment origin of coordinates;
Accompanying drawing 2 is the composition table of comparisons of each embodiment and Comparative Examples;
Accompanying drawing 3 is the soft magnet performance table of comparisons of each embodiment and Comparative Examples.
Embodiment
Come the present invention is further described through the preparation and the Performance Detection of several groups of embodiment and one group of Comparative Examples FINEMT alloy below, but the present invention is not restricted to these embodiment.
In the composition range of iron-based ternary nanocrystals magnetically soft alloy of the present invention, we have prepared many groups embodiment, and the embodiment of the invention and the Comparative Examples composition proportion of 3 groups of wherein representative excellent performances are seen Fig. 2.
The preparation technology and the method for testing performance of embodiment and Comparative Examples are following:
(1) takes by weighing purity greater than 99.9% Fe, P-Fe, Cu, B-Fe, Si-Fe, Nb raw material by the composition proportion of Fig. 2;
(2) raw material for preparing is put into arc furnace, be evacuated to 5 * 10
-3Below the Pa; Earlier the thawing of oxygen uptake Ti piece is exhausted the oxygen in the lumen,residual,, and in the process of melting, apply electromagnetic agitation then repeatedly with each sample melting 4 ~ 5 times; Guarantee uniform component distribution; Then that melted foundry alloy is broken, clean with distilled water, alcohol wash, put into quartz glass tube then.
(3) adopt single roller to revolve the equipment of quenching and prepare amorphous thin ribbon: the quartz glass tube that foundry alloy will be housed is fixed on the running roller top apart from roll surface 1mm place.Be evacuated to 6 * 10
-3Below the Pa, charge into argon gas, the foundry alloy induction heating to high temperature fused state, is cooled off the preparation amorphous thin ribbon through nozzle fast on the copper roller that is ejected into high speed rotating under the pressure effect that argon gas produced, the running roller linear resonance surface velocity is 40m/s.
(4) annealing crystallization legal system is equipped with nano-crystal soft magnetic alloy: the amorphous thin ribbon of fast quenching gained is carried out subsequent annealing under the Ar gas shiled in vacuum annealing furnace.The annealing conditions of embodiment 1 is 300 ℃, temperature retention time 3min; The annealing conditions of embodiment 2 is 350 ℃, temperature retention time 2min; 250 ℃ of the annealing temperatures of embodiment 3, temperature retention time 5min; The annealing conditions of Comparative Examples is 535 ℃, temperature retention time 60min.
(5) insulation is cooled off with stove after finishing.
(6) adopt MATS soft magnetism measuring equipment to test the saturation induction density B of nano-crystal soft magnetic alloy
sWith coercive force H
c, maximum measurement fields 8000A/m, saturation induction density Bs and coercivity H after each embodiment and the Comparative Examples annealing are seen Fig. 3.
As can beappreciated from fig. 2: Fe-based nanocrystalline magnetically soft alloy of the present invention is compared with at present typical FINEMET magnetically soft alloy; Do not contain elements such as valuable Co, Zr, Nb, B; And constituent element ternary only; The existence of a kind of vitrifying element P is only arranged, so alloying component of the present invention there are relative less cost advantage and relatively easy manufacturing advantage.
Can know from Fig. 3: the Bs of Fe-based nanocrystalline magnetically soft alloy of the present invention is up to 1.75T; The minimum 3.5A/m that reaches of coercive force; Though the relative Comparative Examples of coercive force is not very low; But Bs is apparently higher than Comparative Examples for its saturation induction density; It is not to have boundless application space under the very high situation that this Fe-based nanocrystalline magnetically soft alloy system requires at coercive force, is advocating the today that makes up resource-conserving friendly environment society in the whole society at present especially, and this alloy system has immeasurable using value.
This shows that Fe-based nanocrystalline magnetically soft alloy of the present invention has the advantage that constituent element is few, cost is low, soft magnet performance is high, is more suitable for large-scale production, in fields such as electric power electric transformer, instrument transformers wide application prospect is arranged.
Claims (3)
1. the iron-based ternary nanocrystals magnetically soft alloy of a low cost, high soft magnet performance, it is characterized in that: the chemical composition of this nano-crystal soft magnetic alloy can be expressed as Fe
aP
bCu
c, wherein a, b, c represent respectively the atomic percentage of corresponding component, excursion: b=14 ~ 19, c=0.5 ~ 1.5, a=1-b-c.
2. the iron-based ternary nanocrystals magnetically soft alloy of low cost according to claim 1, high soft magnet performance, its characteristic component is: Fe
80P
19Cu
1Or Fe
83P
16.5Cu
0.5Or Fe
84.5P
14Cu
1.5
3. the preparation method of the iron-based ternary nanocrystals magnetically soft alloy of low cost according to claim 1, high soft magnet performance is characterized in that comprising following process:
Step 1, prepare burden and the foundry alloy that is evenly distributed of smelting component according to alloying component;
Step 2, foundry alloy is heated to molten condition, to the copper roller, cools off the preparation amorphous thin ribbon fast through nozzle ejection;
Step 3, the amorphous thin ribbon that fast quenching is obtained are annealed in vacuum annealing furnace, interval 250 ~ 350 ℃ of holding temperature, time 2 ~ 5min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104233121A (en) * | 2014-09-26 | 2014-12-24 | 华南理工大学 | Fe-based amorphous nanocrystalline soft magnetic material and preparing method thereof |
| CN111570819A (en) * | 2020-04-27 | 2020-08-25 | 江苏萌达新材料科技有限公司 | Preparation method of iron-copper-phosphorus alloy diffusion powder |
| CN111575610A (en) * | 2020-06-29 | 2020-08-25 | 华麟津磁（天津）科技有限公司 | SmFeB amorphous soft magnetic alloy material and preparation method thereof |
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| CN101492794A (en) * | 2008-01-21 | 2009-07-29 | 安泰科技股份有限公司 | Iron based amorphous alloy material and uses thereof |
| CN101641455A (en) * | 2007-03-22 | 2010-02-03 | 日立金属株式会社 | Soft magnetic ribbon, magnetic core, magnetic part and process for producing soft magnetic ribbon |
| CN101834046A (en) * | 2009-03-10 | 2010-09-15 | 中国科学院宁波材料技术与工程研究所 | High saturation magnetization intensity Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof |
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2012
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| JPH01156451A (en) * | 1987-12-11 | 1989-06-20 | Hitachi Metals Ltd | Soft-magnetic alloy having high saturation magnetic flux density |
| CN1403615A (en) * | 2002-08-16 | 2003-03-19 | 安泰科技股份有限公司 | Iron-base bulk amorphous soft-magnetic alloy material |
| CN101641455A (en) * | 2007-03-22 | 2010-02-03 | 日立金属株式会社 | Soft magnetic ribbon, magnetic core, magnetic part and process for producing soft magnetic ribbon |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104233121A (en) * | 2014-09-26 | 2014-12-24 | 华南理工大学 | Fe-based amorphous nanocrystalline soft magnetic material and preparing method thereof |
| CN104233121B (en) * | 2014-09-26 | 2016-06-29 | 华南理工大学 | A kind of Fe based amorphous nano soft magnetic materials and preparation method thereof |
| CN111570819A (en) * | 2020-04-27 | 2020-08-25 | 江苏萌达新材料科技有限公司 | Preparation method of iron-copper-phosphorus alloy diffusion powder |
| CN111575610A (en) * | 2020-06-29 | 2020-08-25 | 华麟津磁（天津）科技有限公司 | SmFeB amorphous soft magnetic alloy material and preparation method thereof |
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Application publication date: 20121003 |