CN102610348B - Iron-based nanocrystalline soft magnetic alloy material and preparing method thereof - Google Patents
Iron-based nanocrystalline soft magnetic alloy material and preparing method thereof Download PDFInfo
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Abstract
The invention belongs to the preparation field of soft magnetic materials in functional materials and relates to an iron-based nanocrystalline soft magnetic alloy material and a preparing method thereof. Nanocrystalline is directly formed in rapid solidification process through spinodal decomposition. A general formula of the iron-based nanocrystalline soft magnetic alloy material is Fe100-b-c-d-eCubAcBdCe. Chemical components specifically include (by atom %) b=0.3-3%, c=2-8%, d=10-15% and e=2-15%, wherein the A is at least one of Cr, V, Mo, W, Ta and Nb, the B is at least one of Si and P, and the C is at least one of C and B. By utilizing the spinodal decomposition method, the nanocrystalline soft magnetic alloy material having good soft magnetic performance can be prepared in one step, and the process is simple and quick.
Description
Technical field
The invention belongs to the preparation field of soft magnetic materials in functional material, be particularly useful for making the Fe-based nanocrystalline magnetically soft alloy material with good soft magnet performance.
Background technology
Along with developing rapidly of electron trade, the technical performance index of wherein used various electronic devices and components is also in continuous raising.And adopt crystalline state nanometer alloy as the material of must using of soft magnetic materials, used widely already.
The method of usual acquisition nanometer crystal alloy band has 2 kinds, and a kind of for single-roller method is in conjunction with the heat treated preparation method of follow-up subsequent annealing, another kind is spinodal decomposition method.As everyone knows, single-roller method is the preparation method that current crystalline state nanometer alloy material generally adopts in conjunction with the heat treated preparation method of follow-up subsequent annealing.1988, the Ji Zeke benevolence of Hitachi Metals added Cu and Nb on the basis of Fe-Si-B non-crystaline amorphous metal, utilized single-roller method to obtain non-crystaline amorphous metal, recycled the α-Fe nano-crystalline granule that follow-up crystallization and thermal treatment obtains the diameter 20-50nm of Dispersed precipitate on noncrystal substrate.Wherein, the operation principle of single-roller method is that direct for molten liquid steel spray to the copper roller Quench face rapid solidification of High Rotation Speed is formed non-crystaline amorphous metal, obtained the α-Fe crystal grain of the size 20-50 nanometer of Dispersed precipitate on noncrystal substrate again by follow-up subsequent annealing heat treatment, and this preparation method becomes one of the most important method in order to continuous seepage nanometer crystal alloy strip in recent years.And the operation principle of spinodal decomposition method first makes alloy melt reach deeply undercooling, make it spinodal decomposition occurs, then cooled the alloy strip steel rolled stock obtaining nano-scale by melt fast.Compared with the former, spinodal decomposition method has that technique is simple, a step directly prepares the features such as nanometer crystal alloy.
Summary of the invention
The object of this invention is to provide one and prepare Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof by spinodal decomposition, this preparation method can make the alloying component of proportion optimizing directly form nanometer crystal alloy in rapid solidification, and this alloy material has square than high, the features such as soft magnet performance is good.
Mentality of designing of the present invention is as follows:
Fe-based nanocrystalline magnetically soft alloy material proposed by the invention, is mainly applicable to the material of soft magnetic amorphous alloy, in order to make material have desirable soft magnetic characteristic, and forms nanometer crystal alloy easily through spinodal decomposition, proposes a kind of with Fe
100-b-c-d-ecu
ba
cb
dc
efor the magnetically soft alloy material of basic general formula, and by the Reasonable adjustment of alloy composition, add some other minor metallic element, improve the material behavior of alloy and every magnetic property.
Therefore, in the composition of Fe-based nanocrystalline magnetically soft alloy material of the present invention, adopt Fe as the main composition element of soft magnetic materials, content is 70-85at%.
Being added with of Cu element is beneficial to nanocrystalline formation, and content is 0.3-3at%, is less than 0.3%, not easily forms nano-crystalline granule, and higher than 3%, nano-crystalline granule diameter becomes thick.P, Si, B, C element adds as the important element being conducive to being formed amorphous, wherein, P, Si, B is metalloid element is metalloid element, except can reducing the critical cooling rate of formation non-crystaline amorphous metal, its main effect is conducive to forming non-crystaline amorphous metal, and B can also improve the magnetic property of non-crystaline amorphous metal, such as square ratio, C is metalloid element, it can improve the saturation induction density of non-crystaline amorphous metal, and be conducive to the formation of non-crystaline amorphous metal, wherein C, B content is 2-15at%, lower than 2%, not easily form non-crystaline amorphous metal, higher than 15%, easily cause system band difficulty.The content of Si, P is 10-15at%, lower than 10%, not easily forms non-crystaline amorphous metal, and higher than 15%, alloy not easily forms amorphous band.
Simultaneously, in order to improve the performance of alloy material further, also added the alloy elements such as Cr, V, Mo, W, Ta, Nb, these elements can carry heavy alloyed heat treatment stability, improve the operational characteristic of alloy material when casting, and there is the advantage further expanding alloy degree of supercooling, its content is 2-8at%, and lower than 2%, the degree of supercooling of alloy is too low, higher than 8%, easily cause nanocrystalline formation difficulty.
Fe-based nanocrystalline magnetically soft alloy material of the present invention can adopt single-roller method directly to prepare.
In order to realize goal of the invention, according to above-mentioned mentality of designing, the invention provides following technical scheme:
A kind of Fe-based nanocrystalline magnetically soft alloy material, directly formed nanocrystalline in rapid solidification by spinodal decomposition, wherein, the general formula of this Fe-based nanocrystalline magnetically soft alloy material is Fe
100-b-c-d-ecu
ba
cb
dc
e, concrete chemical analysis is (atom %): b=0.3-3%, c=2-8%, d=10-15%, e=2-15%, wherein A is at least one element in Cr, V, Mo, W, Ta, Nb, B is at least one element in Si, P, and C is at least one element in C, B.
The microstructure of described magnetically soft alloy material using state is: on noncrystal substrate, Dispersed precipitate the α-Fe crystal grain being of a size of 20-50nm.
The square ratio of described magnetically soft alloy material is 0.80-0.94.
A preparation method for Fe-based nanocrystalline magnetically soft alloy material, is directly formed nanocrystalline by spinodal decomposition, it is characterized in that: comprise the steps: in rapid solidification
(1) according to following proportion ingredient, alloy material is Fe
100-b-c-d-ecu
ba
cb
dc
e, concrete chemical analysis is (atom %): b=0.3-3%, c=2-8%, d=10-15%, e=2-15%, wherein A is at least one element in Cr, V, Mo, W, Ta, Nb, B is at least one element in Si, P, and C is at least one element in C, B;
(2) single rod method is adopted to prepare nanometer crystal alloy strip in conjunction with spinodal decomposition: by the raw materials melt in above-mentioned steps (1), molten liquid steel when single-roller method As-deposited state by deeply undercooling generation spinodal decomposition, molten alloy liquid temp remains on 1300 DEG C-1420 DEG C, and molten alloy liquid degree of supercooling remains on 40 DEG C-120 DEG C.
When single-roller method prepares alloy thin band, roller mouth spacing remains on 0.08mm-0.30mm, nozzle mouth seam remains on 0.10mm-0.50mm, molten alloy liquid level remains on 10cm-40cm, chill roll rotating speed remains on 15m/s-40m/s, completes under the condition adding magnetic field, and magnetic field intensity is 1500A/m-2200A/m, magnetic direction is longitudinal magnetic field or magnetic field intensity is 1400A/m-2400A/m, and magnetic direction is transverse magnetic field.
Comprise following crystallization and thermal treatment step further: under the condition adding magnetic field, magnetic field intensity is 1500A/m-2200A/m, and magnetic direction is longitudinal magnetic field, at 540 DEG C-565 DEG C insulation 15-60min.
Compared with prior art, beneficial effect of the present invention is:
Spinodal decomposition method of the present invention is utilized a step can directly to prepare the nanocrystalline magnetically soft alloy material with good soft magnet performance, simple process, quick.
Accompanying drawing explanation
Fig. 1 is the alloy subsides roll surface bright field image of No. 1 alloy material in the first embodiment;
Fig. 2 is the subsides roll surface field trash diffraction pattern of No. 1 alloy material in the first embodiment.
Detailed description of the invention
Below, in conjunction with the embodiments and accompanying drawing, the present invention is further described.
At the compositional ranges of Fe-based nanocrystalline magnetically soft alloy material of the present invention, select the alloy proportion that 12 groups different, wherein, table 1 is alloy sequence number and corresponding alloying component.Then, according to the alloy component range shown in table 1, single-roller method is utilized, adopt different preparation technologies to prepare 12 groups of nanometer crystal alloy materials, and by above-mentioned 12 groups of width 10mm, thickness is at the nano-crystalline thin carry sample of 25-40 μm, be wound into internal diameter 23mm, the circular magnetic core of external diameter 28mm.
Wherein, No. 1, No. 3, No. 5, No. 7 and the preparation of No. 8 alloy materials employing single-roller methods, molten alloy liquid temp remains on 1360 DEG C-1420 DEG C, 1300 DEG C-1360 DEG C are cooled to 5 DEG C-10 DEG C/min, insulation 5min-20min, molten alloy liquid degree of supercooling remains on 40 DEG C-120 DEG C, roller mouth spacing remains on 0.08mm-0.30mm, nozzle mouth seam remains on 0.10mm-0.50mm, molten alloy liquid level remains on 10cm-40cm, complete under the condition adding magnetic field, magnetic field intensity is 1500A/m-2200A/m, magnetic direction is longitudinal magnetic field, namely magnetic direction is for being parallel to zone face injection direction or magnetic field intensity is 1400A/m--2400A/m, magnetic direction is transverse magnetic field, namely magnetic direction is perpendicular to zone face injection direction, chill roll rotating speed remains on 15m/s-40m/s, molten alloy liquid is cast on the chill roll of rotation, it is made when single-roller method As-deposited state, spinodal decomposition to occur, preparation becomes nanometer crystal alloy.As shown in Figures 1 and 2, there is crystallization at single-roller method As-deposited state in No. 1 alloy.Further, as can be seen from SAED (SEAD) figure of Fig. 2, this alloy material is the α-Fe crystal grain that on noncrystal substrate, Dispersed precipitate is of a size of 20-50nm.
First No. 2 alloys adopt single-roller method to prepare, and then under the condition adding magnetic field, magnetic field intensity is 1500A/m-2200A/m, and magnetic direction is longitudinal magnetic field, after 550 DEG C of heat treatment 30min, crystallization occurs, and form nanometer crystal alloy.
First No. 4, No. 6, No. 9, No. 10, No. 11, No. 12 alloys adopt single-roller method to prepare, then under the condition adding magnetic field, magnetic field intensity is 1500A/m-2200A/m, and magnetic direction is longitudinal magnetic field, after 540 DEG C-565 DEG C heat treatment 15min-60min, there is crystallization, form nanometer crystal alloy.
Finally, test the magnetic property of the 12 groups of magnetic cores prepared respectively, result is as shown in table 2-3.From table 2-3, can find out: 2,3,5, No. 12 alloys have comparatively high initial magnetoconductivity, 2,3,5,6,9, No. 12 alloys have lower loss, and 1, No. 3 alloy has the square ratio of higher vertical magnetic.
Table 1 alloying component (atom %)
| Sequence number | Fe | Cu | V | Cr | Mo | W | Ta | Nb | P | Si | B | C |
| No. 1 | 75 | 0.6 | 3 | - | - | - | - | - | - | 11.4 | 10 | - |
| No. 2 | 76 | 1 | 1 | - | - | - | - | 2 | 10 | - | 10 | - |
| No. 3 | 76 | 1 | 2 | - | - | - | 1 | - | 10 | 10 | - | - |
| No. 4 | 71.5 | 1 | 3.5 | 3 | - | - | - | - | - | 12 | 9 | - |
| No. 5 | 71 | 0.5 | 4.5 | 2 | - | - | - | - | 10 | - | 10 | 2 |
| No. 6 | 74 | 1 | - | 2 | 2 | - | - | - | - | 12 | 8 | 1 |
| No. 7 | 74 | 1 | - | 2 | - | 2 | - | - | 10 | 10 | - | 1 |
| No. 8 | 73 | 2 | 3 | - | - | - | - | - | - | 12 | 10 | - |
| No. 9 | 73 | 1 | 3 | - | 3.5 | - | - | - | - | 10 | 8 | 1.5 |
| No. 10 | 78 | 1 | 1 | 4 | - | - | - | - | 10 | 6 | - | - |
| No. 11 | 71 | 2.5 | 5.5 | 1 | - | - | - | - | 8 | 4 | 4 | 2 |
| No. 12 | 74 | 1 | - | - | 1.5 | - | - | 1.5 | 10 | 4 | 4 | 4 |
Show 2-in-1 gold and magnetic property
Table 3 alloy and magnetic property
Claims (6)
1. a Fe-based nanocrystalline magnetically soft alloy material, is directly formed nanocrystalline by spinodal decomposition, it is characterized in that: the general formula of this Fe-based nanocrystalline magnetically soft alloy material is Fe in rapid solidification
100-b-c-d-ecu
ba
cb
dc
e, concrete chemical analysis is (atom %): b=0.3-3%, c=2-8%, d=10-15%, e=2-15%, wherein A is at least one element in Cr, V, Mo, W, Ta, Nb, B is at least one element in Si, P, and C is at least one element in C, B;
This Fe-based nanocrystalline magnetically soft alloy material is prepared by following preparation method: according to proportion ingredient; Single-roller method is adopted to prepare nanometer crystal alloy strip in conjunction with spinodal decomposition: by above-mentioned raw materials melting, molten alloy liquid when single-roller method As-deposited state by deeply undercooling generation spinodal decomposition, molten alloy liquid temp remains on 1300 DEG C-1420 DEG C, and molten alloy liquid degree of supercooling remains on 40 DEG C-120 DEG C.
2. Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 1, is characterized in that: the microstructure of described magnetically soft alloy material using state is: on noncrystal substrate, Dispersed precipitate the α-Fe crystal grain being of a size of 20-50nm.
3. Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 1, is characterized in that: the square ratio of described magnetically soft alloy material is 0.80-0.94.
4. a preparation method for Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 1, is directly formed nanocrystalline by spinodal decomposition, it is characterized in that: comprise the steps: in rapid solidification
(1) according to following proportion ingredient, alloy material is Fe
100-b-c-d-ecu
ba
cb
dc
e, concrete chemical analysis is (atom %): b=0.3-3%, c=2-8%, d=10-15%, e=2-15%, wherein A is at least one element in Cr, V, Mo, W, Ta, Nb, B is at least one element in Si, P, and C is at least one element in C, B;
(2) single-roller method is adopted to prepare nanometer crystal alloy strip in conjunction with spinodal decomposition: by the raw materials melt in above-mentioned steps (1), molten alloy liquid when single-roller method As-deposited state by deeply undercooling generation spinodal decomposition, molten alloy liquid temp remains on 1300 DEG C-1420 DEG C, and molten alloy liquid degree of supercooling remains on 40 DEG C-120 DEG C.
5. the preparation method of Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 4, it is characterized in that: when single-roller method prepares alloy thin band, roller mouth spacing remains on 0.08mm-0.30mm, nozzle mouth seam remains on 0.10mm-0.50mm, molten alloy liquid level remains on 10cm-40cm, chill roll rotating speed remains on 15m/s-40m/s, complete under the condition adding magnetic field, magnetic field intensity is 1500A/m-2200A/m, magnetic direction is longitudinal magnetic field or magnetic field intensity is 1400A/m-2400A/m, and magnetic direction is transverse magnetic field.
6. the preparation method of Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 4, it is characterized in that: comprise following crystallization and thermal treatment step further: under the condition adding magnetic field, magnetic field intensity is 1500A/m-2200A/m, magnetic direction is longitudinal magnetic field, at 540 DEG C-565 DEG C insulation 15-60min.
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| US20190055635A1 (en) * | 2017-08-18 | 2019-02-21 | Samsung Electro-Mechanics Co., Ltd. | Fe-based nanocrystalline alloy and electronic component using the same |
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| JP7043877B2 (en) * | 2018-02-21 | 2022-03-30 | Tdk株式会社 | Soft magnetic alloys and magnetic parts |
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