CN104831169A - Fe-based nano crystal soft magnetic alloy material and preparation method thereof - Google Patents
Fe-based nano crystal soft magnetic alloy material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a Fe-based nano crystal soft magnetic alloy material and a preparation method thereof. A molecular formula of the material is FeaNbbBcCud, wherein, a, b, c and d respectively present atom percentage content of corresponding elements, a is greater than or equal to 80 and less than or equal to 85, b is greater than or equal to 1 and less than or equal to 3, c is greater than or equal to 12 and less than or equal to 18, d is greater than or equal to 0.8 and less than or equal to 1.2, wherein, sum of a, b, c and d is 100. The alloy material has high Fe element content and low Nb element content, production cost is reduced; a structure comprises an amorphous matrix and an alpha-Fe NANO crystal grain phase with average crystal grain size less than 20nm body-centered cubic, the alloy material has high saturation magnetic induction intensity and low coercive force, so that the Fe-based nano crystal soft magnetic alloy material has the advantages of low cost and good soft-magnetic performance, and has good application prospect.
Description
Technical field
The present invention relates to Fe-based nanocrystalline magnetically soft alloy material technical field, particularly relate to one and there is low cost, Fe-based nanocrystalline magnetically soft alloy material of high saturated magnetic induction, low-coercivity and preparation method thereof.
Background technology
Fe-based amorphous, nano-crystal soft magnetic alloy has the excellent properties such as high saturation induction density, high-strong toughness, low-loss, low-coercivity, high magnetic permeability, its preparation technology is simple simultaneously, with low cost, energy-efficient, product energy-conserving and environment-protective, miniaturization, lightweight development can be promoted, in electric power mutual-inductor, power transformer etc., there is widespread use.
Fe-based nanocrystalline magnetically soft alloy is prepared through crystallization and thermal treatment by non-crystaline amorphous metal, and alloy structure is made up of noncrystal substrate and nanocrystal two phase structure, has therefore had the multiple advantages of traditional crystalline state soft magnetic materials and amorphous soft magnetic material concurrently.Up to the present, the research of iron based nano crystal soft magnetism mainly comprises three individual system: Fe-Si-B-M-Cu (M=Nb, Mo, W, Ta etc.) FINMET system alloy, Fe-M-B-Cu (M=Zr, Hf, Nb etc.) NANOPERM system's alloy and (Fe, Co)-M-B-Cu (M=Zr, Hf, Nb etc.) are HITPERM system alloy.
Wherein, the comprehensive soft magnetic performance of FINEMET system alloy is more excellent, has high magnetic permeability, the features such as low-loss, because alloy saturation induction density size depends on Fe content, its Fe constituent content is lower, non-metallic element Si and B equal size higher, cause saturation induction density lower, typical composition Fe
73.6nb
3si
13.5b
9cu
1saturation induction density be only 1.24T.
Compared with FINEMET, NANOPERM system and HITPERM system alloy show higher saturation induction density, and alloy magnetostriction coefficient levels off to zero, greatly reduces its stress sensitivity, can use in high frequency.But, the existence of a large amount of oxidizable expensive metal Zr, Hf etc., and more containing a large amount of Co elements in HITPERM, result in cost of alloy and improve, make complicated process of preparation simultaneously.
Current electron electric power, military civilian industry field, the magnetic devices such as high-frequency inductor, high frequency switch power, high-frequency transformer progressively carry out lightweight, miniaturization, high-tension transmission line requirements increases increasingly, the energy saving and environment friendly development of society and nature's environmental requirement industrial production, one to appear is had to have high saturated magnetic induction, the good and Fe-based nanocrystalline magnetically soft alloy material of low production cost of soft magnetic performance.
Summary of the invention
Technical problem to be solved by this invention is, a kind of Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof is provided, this material iron level is higher, expensive metal and nonmagnetic constituent content less, low production cost, and the advantage with the good soft magnetic performance such as high saturated magnetic induction and low-coercivity.
The molecular formula of Fe-based nanocrystalline magnetically soft alloy material provided by the invention is:
Fe
aNb
bB
cCu
d
Wherein, a, b, c, d represent the atomic percentage conc of each corresponding element respectively, 80≤a≤85,1≤b≤3,12≤c≤18,0.8≤d≤1.2, and a+b+c+d=100.
As preferably, described 80≤a≤85, more preferably 82≤a≤84.
As preferably, described 1≤b≤3, more preferably 1.5≤b≤2.5.
As preferably, described 12≤c≤18, more preferably 13≤c≤16.
As preferably, described 0.8≤d≤1., more preferably 0.9≤d≤1.1.
Present invention also offers a kind of method preparing above-mentioned Fe-based nanocrystalline magnetically soft alloy material, comprise the steps:
Step 1: take each element according to above-mentioned molecular formula and prepare burden;
Step 2: raw material step 1 prepared loads in smelting furnace, carries out melting, obtain the mother alloy ingot of uniform composition after cooling under inert atmosphere protection;
Step 3: mother alloy ingot is broken for fritter sample, adopts single roller to get rid of the obtained non-crystaline amorphous metal of band again after melting;
Step 4: non-crystaline amorphous metal is carried out Annealing Crystallization process, obtains nanocrystalline magnetically soft alloy material.
As preferably, in described step 1, the purity of element of Fe, Nb, B and Cu is all not less than 99wt.%.
As preferably, in described step 2, smelting temperature is 1300-1800 DEG C.
As preferably, in described step 2, smelting time is 20-40 minute.
As preferably, in described step 3, non-crystaline amorphous metal is ribbon, and strip width is preferably 1-2mm, and thickness is preferably 20-25 μm.
As preferably, in described step 4, Annealing Crystallization treating processes is: non-crystaline amorphous metal is carried out Crystallizing treatment by isothermal annealing in vacuum atmosphere, is then quenched to room temperature.
As preferably, in described step 4, annealing temperature is 530-570 DEG C.
As preferably, in described step 4, annealing time is 1-3 minute, more preferably 2.5-3.5 minute.
Compared with prior art, beneficial effect of the present invention is as follows:
In sum, the present inventor is based on the long-term research practice in amorphous magnetic material technical field, in conjunction with the state of the art of existing amorphous magnetic alloy, by a large amount of experiment repeatedly, obtain the component content formula of the Fe-based nanocrystalline magnetically soft alloy that the present invention proposes, utilize this formula to carry out preparing burden the Fe-based nanocrystalline magnetically soft alloy for preparing while possessing stronger amorphous formation ability and magnetic property, there is outstanding breaking tenacity and plastic deformation ability.Compared with existing amorphous magnetic alloy, amorphous magnetic alloy specific performance advantage provided by the invention is as follows:
(1) in the present invention, Fe-based nanocrystalline magnetically soft alloy material is elementary composition by Fe, Nb, B, Cu, wherein, Fe constituent content is higher, and atomic percentage conc is in 80-85 scope, and the content of Nb element is lower, atomic percentage conc, in 1-2.5 scope, therefore greatly reduces the cost of alloy material; The structure of this Fe-based nanocrystalline magnetically soft alloy material comprises noncrystal substrate and nanocrystal phase, and this nanocrystal is body-centred cubic α-Fe mutually, and its grain-size mean value is less than 20nm; Meanwhile, this Fe-based nanocrystalline magnetically soft alloy material has good magnetic property, not only has high saturation induction density, also have lower coercive force, its saturation induction density is at more than 1.6T, and coercive force is lower than 20A/m, preferably lower than 12A/m, even can control in 5-10A/m scope;
(2) method of this nanocrystalline magnetically soft alloy material of preparation provided by the invention is simple to operation, obtained alloy material structure comprises noncrystal substrate and nanometer crystalline phase, Educt of crystals is body-centred cubic α-Fe, and nanocrystalline grain size mean value is less than 20nm;
Therefore, Fe-based nanocrystalline magnetically soft alloy material of the present invention has the advantage of low cost, high soft magnetic performance, has a good application prospect, such as, can be applicable to the technical fields such as annular core, transformer and aerospace.
Accompanying drawing explanation
Fig. 1 is Fe in the embodiment of the present invention 1
83nb
2b
14cu
1x-ray diffraction (XRD) collection of illustrative plates of alloy strip non-crystalline state and crystalline state nanometer;
Fig. 2 is the state Fe that quenches in the embodiment of the present invention 1
83nb
2b
14cu
1the DSC curve of amorphous alloy strips;
Fig. 3 is the Fe in the embodiment of the present invention 1 after thermal treatment
83nb
2b
14cu
1the room temperature magnetic hysteresis loop of nanometer crystal alloy band;
Fig. 4 is the Fe in the embodiment of the present invention 1 after thermal treatment
83nb
2b
14cu
1the transmission electron microscope bright field image of nanometer crystal alloy band and selected area electron diffraction image;
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail, it is pointed out that the following stated embodiment is intended to be convenient to the understanding of the present invention, and any restriction effect is not play to it.
Embodiment 1:
In the present embodiment, the molecular formula of Fe-based nanocrystalline magnetically soft alloy material is Fe
83nb
2b
14cu
1.
The preparation method of this Fe-based nanocrystalline magnetically soft alloy material is as follows:
(1) purity is greater than the iron of 99%, cobalt, niobium, boron, copper raw material according to molecular formula Fe
83nb
2b
14cu
1shown component atoms per-cent is prepared burden;
(2) raw material step 1 prepared loads in arc-melting furnace, and arc melting 5 times, obtains the alloy pig of uniform composition;
(3) by filling after alloy pig fragmentation in right amount in silica tube, adopting single roller chilling to get rid of band technology, getting rid of band with the speed of 40m/s in an ar atmosphere, obtained AMORPHOUS ALLOY RIBBONS;
(4) AMORPHOUS ALLOY RIBBONS is placed in silica tube, is evacuated to lower than 3 × 10
-3pa, is then placed in heat treatment furnace, and silica tube was put into quenching-in water to room temperature rapidly after 3 minutes by 540 DEG C of insulations, obtained nanometer crystal alloy material.
The XRD figure spectrum of quench state alloy strip and the alloy strip after step (4) thermal treatment that adopt D8Advance type polycrystal X ray diffractometer test procedure (3) obtained, result as shown in Figure 1, visible, state of quenching band is non-crystal structure, alloy bar after thermal treatment is with obvious crystallization peak, the inner crystallization of alloy is described, this Crystallization Phases is body-centred cubic α-Fe phase by analysis, estimates that its grain-size is about 16nm by Scherrer formula.
The DSC curve of the state alloy strip of quenching adopting NETZSCH DSC 404C differential scanning calorimeter measuring process (3) obtained, temperature rise rate arranges 40 DEG C/min, and result as shown in Figure 2, records the initial crystallization temperature T of AMORPHOUS ALLOY RIBBONS
x1be 413 DEG C, secondary crystallization temperature T
x2it is 557 DEG C.
Adopt vibrating sample magnetometer (VSM, Lakeshore7410) magnetic hysteresis loop of the nanometer crystal alloy band after step (4) thermal treatment is measured, DC magnetizing characteristic analyser (B-H Curve Tracer, EXPH-100) is adopted to measure the coercive force of the nanometer crystal alloy band after step (4) thermal treatment.As shown in Figure 3, the saturation magnetization recording this alloy is 1.7T to test result, and coercive force is 7A/m.
Adopt microtexture and the selected area electron diffraction figure of the alloy strip of TecnaiF20 type transmission electron microscope observation after step (4) thermal treatment, result as shown in Figure 4, can find out, this nanometer crystal alloy structure comprises noncrystal substrate and nanocrystal, grain size distribution is even, obtaining separating out crystal grain through measuring and calculating is α-Fe phase, and size is about 16nm, and XRD analysis result is coincide.
Above-described embodiment has carried out system detailed description to technical solution of the present invention, is understood that described example is only specific embodiments of the invention, is not limited to the present invention.All make in spirit of the present invention any amendment, supplement or equivalent to replace, all should be included within protection scope of the present invention.
Claims (9)
1. Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof, its molecular formula is:
Fe
aNb
bB
cCu
d
Wherein, a, b, c, d represent the atomic percentage conc of each corresponding element respectively, 80≤a≤85,1≤b≤3,12≤c≤18,0.8≤d≤1.2, and a+b+c+d=100.
2. a kind of Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 1 and preparation method thereof, is characterized in that: 80≤a≤85, is preferably 82≤a≤83.5.
3. a kind of Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 1 and preparation method thereof, is characterized in that: 1≤b≤3, is preferably 1.5≤b≤2.5.
4. a kind of Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 1 and preparation method thereof, is characterized in that: 12≤c≤18, is preferably 13≤c≤16.
5. a kind of Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 1 and preparation method thereof, is characterized in that: 0.8≤d≤1.2, is preferably 0.9≤d≤1.1.
6. a kind of Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 1 and preparation method thereof, it is characterized in that: its nanocrystalline structure comprises noncrystal substrate and nanocrystal phase, described nanocrystal is body-centred cubic α-Fe mutually, and its average grain size is less than 20nm.
7. a kind of Fe-based nanocrystalline magnetically soft alloy material as described in claim arbitrary in claim 1 to 6 and preparation method thereof, is characterized in that: saturation induction density is at more than 1.6T, and coercive force is at below 20A/m.
8. a kind of Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 1 and preparation method thereof, is characterized in that: coercive force, at below 20A/m, is preferably 5-15A/m.
9. a kind of Fe-based nanocrystalline magnetically soft alloy material as described in claim arbitrary in claim 1 to 6 and preparation method thereof, is characterized in that: comprise the following steps:
Step 1: take each element according to described molecular formula and prepare burden;
Step 2: raw material step 1 prepared loads in smelting furnace, carries out melting, obtain the mother alloy ingot of uniform composition after cooling under inert atmosphere protection; As preferably, smelting temperature is 1200-1700 DEG C;
Step 3: mother alloy ingot is broken for fritter sample, adopts single roller to get rid of the obtained non-crystaline amorphous metal of band again after melting; As preferably, non-crystaline amorphous metal is width is 1-1.5mm, and thickness is the ribbon of 20-25 μm;
Step 4: non-crystaline amorphous metal is carried out Annealing Crystallization process, obtains nanocrystalline magnetically soft alloy material; As preferably, annealing temperature is 530-570 DEG C; As preferably, annealing time is 2.5-3.5 minute.
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| CN105755356A (en) * | 2016-03-15 | 2016-07-13 | 梁梅芹 | Preparation method of iron-based nanocrystalline soft magnetic alloy |
| CN105903951A (en) * | 2016-05-23 | 2016-08-31 | 苏州思创源博电子科技有限公司 | Preparation method of magnetically soft alloy powder |
| CN108220768A (en) * | 2016-12-15 | 2018-06-29 | 三星电机株式会社 | Fe Based Nanocrystalline Alloys, the electronic building brick using it and the method that manufactures it |
| CN109754975A (en) * | 2019-03-14 | 2019-05-14 | 安徽智磁新材料科技有限公司 | Nanometer crystal alloy and preparation method thereof with excellent toughness |
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| CN110257721A (en) * | 2019-07-01 | 2019-09-20 | 济南大学 | A kind of Fe base magnetically soft alloy of lower Fe content and its preparation method and application |
| CN112442642A (en) * | 2019-09-03 | 2021-03-05 | 真空融化股份有限公司 | Metal strip, method for producing an amorphous metal strip and method for producing a nanocrystalline metal strip |
| CN113046657A (en) * | 2021-03-01 | 2021-06-29 | 青岛云路先进材料技术股份有限公司 | Iron-based amorphous nanocrystalline alloy and preparation method thereof |
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Cited By (12)
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| CN105671460A (en) * | 2016-01-19 | 2016-06-15 | 西安工业大学 | Preparation method for low-cost FeNbB ternary amorphous alloy soft magnetic material |
| CN105671460B (en) * | 2016-01-19 | 2017-07-11 | 西安工业大学 | The preparation method of inexpensive FeNbB ternarys non-crystaline amorphous metal soft magnetic materials |
| CN105755356A (en) * | 2016-03-15 | 2016-07-13 | 梁梅芹 | Preparation method of iron-based nanocrystalline soft magnetic alloy |
| CN105903951A (en) * | 2016-05-23 | 2016-08-31 | 苏州思创源博电子科技有限公司 | Preparation method of magnetically soft alloy powder |
| CN108220768A (en) * | 2016-12-15 | 2018-06-29 | 三星电机株式会社 | Fe Based Nanocrystalline Alloys, the electronic building brick using it and the method that manufactures it |
| CN109754975A (en) * | 2019-03-14 | 2019-05-14 | 安徽智磁新材料科技有限公司 | Nanometer crystal alloy and preparation method thereof with excellent toughness |
| CN110029291A (en) * | 2019-05-23 | 2019-07-19 | 西安工业大学 | A kind of iron base amorphous magnetically-soft alloy and preparation method thereof |
| CN110257721A (en) * | 2019-07-01 | 2019-09-20 | 济南大学 | A kind of Fe base magnetically soft alloy of lower Fe content and its preparation method and application |
| CN112442642A (en) * | 2019-09-03 | 2021-03-05 | 真空融化股份有限公司 | Metal strip, method for producing an amorphous metal strip and method for producing a nanocrystalline metal strip |
| US12077833B2 (en) | 2019-09-03 | 2024-09-03 | Vacuumschmelze Gmbh & Co. Kg | Metal strip, method for producing an amorphous metal strip and method for producing a nanocrystalline metal strip |
| CN113046657A (en) * | 2021-03-01 | 2021-06-29 | 青岛云路先进材料技术股份有限公司 | Iron-based amorphous nanocrystalline alloy and preparation method thereof |
| CN115992334A (en) * | 2022-12-28 | 2023-04-21 | 广东咏旺新材料科技有限公司 | Iron-based amorphous/nanocrystalline material with high Bs, and preparation method and application thereof |
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