CN104485192A - Iron-based amorphous nano-crystal soft magnetic alloy and preparation method thereof - Google Patents
Iron-based amorphous nano-crystal soft magnetic alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an iron-based amorphous nano-crystal soft magnetic alloy and a preparation method thereof. The method comprises the following steps: first proportioning chemical compositions of a mother alloy raw material in percentage by weight: 7-10% of Si, 1.8-2.2% of B, 1-1.5% of Cu, 4-6% of Nb and the balance of Fe; repeatedly melting the mother alloy raw material and casting the mother alloy raw material into an alloy ingot; crushing the alloy ingot, remelting the crushed alloy ingot and covering with a steelmaking fluxing medium; preparing an amorphous thin band by use of a single-roll quenching band preparation method; putting the obtained amorphous thin band into a vacuum annealing furnace and performing isothermal annealing crystallization treatment; then performing furnace cooling to a room temperature, thereby obtaining the iron-based amorphous nano-crystal soft magnetic alloy. By virtue of combination of low-cost industrial raw materials used as raw materials and the preparation method disclosed by the invention, the iron-based amorphous nano-crystal soft magnetic alloy has the characteristics of low cost and high magnetic permeability.
Description
Technical field
The present invention belongs to magnetic material and preparing technical field thereof, especially relates to low-loss Fe-based nanocrystalline magnetically soft alloy of a kind of high permeability and preparation method thereof.
Background technology
Along with social development, in fields such as electric power system, computer network, multimedia technology and high frequency micro-magnetic device, more and more require components and parts high-quality used, small-sized, light weight, this just requires that the Metallic Functional Materials such as used magnetically soft alloy improve constantly performance, and namely this soft magnetic material will have both high saturation and magnetic intensity (Bs) and high permeability (μ) simultaneously.The discovery of " Finemet " nano-crystal soft magnetic alloy is the breakthrough solving this difficult problem.This magnetically soft alloy has high saturation and magnetic intensity (Bs: 1.24T), high initial magnetic permeability (μ
0: 8 x 10
4gs/Oe), low iron loss (Ps
0.5/20k: 20W/kg) etc. characteristic, be widely used.
The Exemplary chemical composition of " Finemet " nano-crystal soft magnetic alloy is Fe
73.5cu
1nb
3si
13.5b
9its preparation principle first prepares amorphous alloy strips by fast solidification technology, then after suitable temperature subsequent annealing, amorphous and Nanocrystalline Two-phase structure is formed, wherein Cu segregation is separated out in advance, carry out forming core again at Cu cluster periphery α-FeSi, therefore Cu has the effect promoting forming core; And Nb discharges from α-FeSi crystal grain, enrichment in residue amorphous phase, and stable residue amorphous phase, thus there is the effect of inhibiting grain growth.In existing iron-base nanometer crystal alloy, Nb is indispensable element, and content is greater than 5% usually, but Nb's is expensive, Nb element occupies more than 70% of raw material total cost, and this causes the cost of raw material of iron-base nanometer crystal alloy very high, is unfavorable for suitability for industrialized production.
Chinese invention patent CN 1621550A discloses a kind of Fe
76.5-x-y-zcu
1nb
xv
ysi
zb
9(atomic ratio) Fe-based nanocrystalline magnetically soft alloy, and 0 < X < 5,0 < Y < 7,0 < Z < 20, use V Some substitute Nb.This invention Fe-based nanocrystalline magnetically soft alloy can have special squareness ratio without magnetic field process and can reduce the cost of raw material, but, relative Fe
73.5si
13.5b
9cu
1nb
3nano-crystal soft magnetic alloy, the permeability of such Fe-based nanocrystalline magnetically soft alloy declines, and coercive force rises.
Open CN 103187136 A of Chinese invention patent discloses a kind of Fe-based amorphous soft magnetic material, and this material is Fe
ay
bsi
cb
d(atomic ratio), wherein a, b, c, d are respectively the atom percentage content of corresponding constituent element, a+b+c+d=100, and 72≤a≤78,1≤b≤5,8≤c≤10,11≤d≤14.Its advantage is: Fe
ay
bsi
cb
dthe non-crystaline amorphous metal of system has larger amorphous formation ability, excellent saturation induction density, low-coercivity and high initial permeability.The preferred constitutional chemistry composition of described material is Fe
77y
1si
9b
13and Fe
76y
2si
9b
13(atomic ratio), its saturation induction density is respectively 1.67 T and 1.60 T, but coercive force, the parameter such as permeability and loss of this material are not mentioned.Further, due to adding of oxidizable Rare Earth Y, make complicated process of preparation, be unfavorable for suitability for industrialized production.
Chinese invention patent CN 101834046A discloses a kind of high saturated magnetic induction Fe-based nanocrystalline magnetically soft alloy and preparation method thereof, it is characterized in that it is the Fe be made up of iron, silicon, boron, phosphorus, copper
xsi
yb
zp
acu
balloy, in formula, x, y, z, a, b represent the atom percentage content of each corresponding component respectively, wherein x=70-90%, y=1-15%, z=1-20%, a=1-20%, b=0.1-1%, and x+y+z+a+b=100%; The micro-structural of this Fe-based nanocrystalline magnetically soft alloy is the body-centered cubic α-Fe(Si of size between 1-35nm) nanometer crystalline phase coexists with the amorphous phase being rich in phosphorus and boron, and is matrix phase with amorphous phase.The raw material that proportioning is good is mainly first prepared into alloy pig by preparation method, then makes non-crystaline amorphous metal, then carries out the process of other operation, finally obtains the Fe-based nanocrystalline magnetically soft alloy of high saturation and magnetic intensity.This invention significantly can improve the saturation magnetization of nano-crystal soft magnetic alloy, can keep lower coercive force simultaneously and effectively reduce the cost of raw material.But the interpolation of P can cause alloy to be easily oxidized in preparation process, collapse and spatter, alloying component is wayward, is unfavorable for suitability for industrialized production, and the relative Fe of gained nano crystal soft magnetic material
73.5si
13.5b
9cu
1nb
3nanometer crystal alloy coercive force rises.
Summary of the invention
The object of the invention is the deficiency in order to overcome above-mentioned existing existence and high permeability low-loss iron-based amorphous and nanocrystalline soft magnetic alloy that a kind of high-performance, low cost are provided and preparation method thereof.
Object of the present invention can be achieved through the following technical solutions: according to object of the present invention, we are applicable industrial mass production by the iron-based amorphous and nanocrystalline soft magnetic alloy FeSiBCuNb object designed by optimization of Chemical Composition, the cost lower than iron-based amorphous and nanocrystalline soft magnetic alloy of the prior art should be possessed, the features such as higher permeability and lower loss.Raw material used in the present invention is the raw material of industry of low cost, prior art uses raw material of the present invention cannot obtain standard compliant iron-based amorphous and nanocrystalline soft magnetic alloy, use the present invention can prepare the iron-based amorphous and nanocrystalline soft magnetic alloy of high magnetic conductivity and low loss low cost, it is characterized in that the specific chemical composition percentage by weight of this alloy material is: Si 7 ~ 10; B 1.8 ~ 2.2; Cu 1.0 ~ 1.5; Nb 4 ~ 6; Surplus is Fe, and one to be in the present invention used in industrial iron-based amorphous and nanocrystalline soft magnetic alloy material composition preferably Nb content lower than 5.66%.
The present invention also provides a kind of and aims at the method manufacturing iron-based amorphous and nanocrystalline soft magnetic alloy of the present invention, and the method comprises the following steps:
(1) proportioning foundry alloy raw material: raw material all adopt more easily starts with and the cheaper existing industrial raw material of price, as Armco iron, Commercial multicrystalline silicon, industrial ferro-boron, industrial ferro-niobium, cathode copper.By industrial raw materials, according to chemical composition (weight ratio) is made into composition is Si 7 ~ 10; B 1.8 ~ 2.2; Cu 1.0 ~ 1.5; Nb 4 ~ 6; Surplus is Fe, wherein, and Nb weight preferably 4 ~ 5.66%;
(2) foundry alloy melting: 1. foundry alloy raw material good for proportioning is positioned over mid-frequency melting furnace in top by the order of a small amount of Armco iron-industrial ferro-niobium, a small amount of industrial ferro-boron-a small amount of Armco iron, cathode copper, surplus industry ferro-boron-a small amount of Armco iron, Commercial multicrystalline silicon, surplus Armco iron from bottom smelting furnace, keeps mid-frequency melting furnace initial power 20-40kW;
2. when step 1. in foundry alloy material temperature reach 300-380 spend time, power rises to 80-100kW;
3. when step 2. in bottom smelting furnace the temperature of foundry alloy raw material reach 1100-1535 spend time, foundry alloy raw material starts to melt and foundry alloy raw material integral sinking, and mid-frequency melting furnace power rises to 140-160kW;
4. when 3. middle foundry alloy raw material melts step completely, stop heating, steelmaking slag agent be covered in anti-oxidation on alloy molten solution and remove the gred, keeping after 5-10 minute, slag former is removed clean;
5. turn forward the alloy solution after step 4. melting 15-20 °, and regulate mid-frequency melting furnace power to 30-40kW, keep 1-2 minute, rapidly power is risen to 100-120kW, alloy molten solution is rolled in smelting furnace, keep again power being down to 30-40kW after 3-5 minute, repeat this step 3-5 time;
6. after 5. step has operated, stop heating, alloy molten solution steelmaking slag agent covers anti-oxidation and removes the gred, retention time 5-10 minute, is removed by slag former clean, and after repeating 3-5 time, alloy molten solution casting is come out of the stove, obtained master alloy ingot;
(3) amorphous thin ribbon is prepared: the master alloy ingot first step (2) prepared is broken, add the Frequency Induction Heating melting refusion in the stove of pocket builder, in process, alloy molten solution steelmaking slag agent covers anti-oxidation, remove clean before system band, then, under atmospheric environment, adopt single roller chilling band method that the alloy molten solution of remelting is prepared into amorphous thin ribbon;
(4) nano-crystallization process: the amorphous thin ribbon that step (3) obtains is put into vacuum annealing furnace and carries out isothermal annealing Crystallizing treatment;
The preferred strip width 10mm of Fe-based amorphous nanocrystalline alloy prepared by the present invention, thickness of strip 30 μm.
Isothermal annealing Crystallizing treatment technique is carried out in preferred steps (4) nano-crystallization process in vacuum annealing furnace: 480-500 degree preannealing 60 minutes, 500-550 DEG C of subsequent annealing 90 minutes, is quickly cooled to less than 350 DEG C to come out of the stove then to carry out air-cooled to room temperature after heat treatment.
A kind of iron-based amorphous and nanocrystalline soft magnetic alloy in the present invention on the basis of traditional soft magnetic alloy, carries out optimizing components have chosen Fe, Si, B, Cu, Nb five elements, and the content reducing Nb realizes reducing material cost; In addition, the raw material prepared in the present invention required for foundry alloy all adopt industrial raw material, prepare iron base amorphous magnetically-soft alloy, reduce material cost simultaneously, be more conducive to industrial mass production with the use of method of the present invention.Further, low cost, high permeability and low-loss iron-based amorphous and nanocrystalline soft magnetic alloy is prepared.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
The chemical composition of foundry alloy is: Fe 81.75, Si 9.56, B 1.94, Cu 1.38, Nb 5.37(wt%).First the melting under atmospheric environment of Frequency Induction Heating smelting furnace is adopted to prepare foundry alloy.Secondly foundry alloy carries out remelting under the protection of steel-making slag former, and removes clean before system band.Again, under atmospheric environment, adopt single roller chilling band to equip and be prepared into amorphous alloy ribbon.Strip width 10mm, thickness of strip 30 μm, toughness is good, to constantly curved.Amorphous thin ribbon is wound into the magnetic core being of a size of 13.2 × 21.5 × 10 mm.Finally in vacuum annealing furnace, carry out isothermal annealing Crystallizing treatment, optimum treatment process is: 480 degree of preannealings 60 minutes, 500 DEG C of subsequent annealings 90 minutes, be quickly cooled to less than 350 DEG C to come out of the stove after heat treatment then to carry out air-cooled to room temperature, during the effective permeability μ e(H=0.05A/m of obtained magnetic core under 1kHz condition) be greater than 140,000 Gs/Oe, loss P under 20kHz, 0.2T condition
0.2/20k=3.6 W/kg.
Embodiment 2
The chemical composition of foundry alloy is: Fe 82.18, Si 9.25, B 1.94, Cu 1.37, Nb 5.26(wt%).First the melting under atmospheric environment of Frequency Induction Heating smelting furnace is adopted to prepare foundry alloy.Secondly foundry alloy carries out remelting under the protection of steel-making slag former, and removes clean before system band.Again, under atmospheric environment, adopt single roller chilling band to equip and be prepared into amorphous alloy ribbon.Strip width 10mm, thickness of strip 30 μm, toughness is good, to constantly curved.Amorphous thin ribbon is wound into the magnetic core being of a size of 13.2 × 21.5 × 10 mm.Finally in vacuum annealing furnace, carry out isothermal annealing Crystallizing treatment, optimum treatment process is: 500 degree of preannealings 60 minutes, 550 DEG C of subsequent annealings 90 minutes, be quickly cooled to less than 350 DEG C to come out of the stove after heat treatment then to carry out air-cooled to room temperature, during the effective permeability μ e(H=0.05A/m of obtained magnetic core under 1kHz condition) be greater than 120,000 Gs/Oe, loss P under 20kHz, 0.2T condition
0.2/20k=4.2 W/kg.
Embodiment 3
The chemical composition of foundry alloy is: Fe 81.67, Si 9.56, B 1.94, Cu 1.38, Nb 5.46(wt%).First the melting under atmospheric environment of Frequency Induction Heating smelting furnace is adopted to prepare foundry alloy.Secondly foundry alloy carries out remelting under the protection of steel-making slag former, and removes clean before system band.Again, under atmospheric environment, adopt single roller chilling band to equip and be prepared into amorphous alloy ribbon.Strip width 10mm, thickness of strip 30 μm, toughness is good, to constantly curved.Amorphous thin ribbon is wound into the magnetic core being of a size of 13.2 × 21.5 × 10 mm.Finally in vacuum annealing furnace, carry out isothermal annealing Crystallizing treatment, optimum treatment process is: 480 degree of preannealings 60 minutes, 550 DEG C of subsequent annealings 90 minutes, be quickly cooled to less than 350 DEG C to come out of the stove after heat treatment then to carry out air-cooled to room temperature, during the effective permeability μ e(H=0.05A/m of obtained magnetic core under 1kHz condition) be greater than 130,000 Gs/Oe, loss P under 20kHz, 0.2T condition
0.2/20k=4.0 W/kg.
Embodiment 4
The chemical composition of foundry alloy is: Fe 82.094, Si 9.246, B 1.935, Cu 1.373, Nb 5.352(wt%).First the melting under atmospheric environment of Frequency Induction Heating smelting furnace is adopted to prepare foundry alloy.Secondly foundry alloy carries out remelting under the protection of steel-making slag former, and removes clean before system band.Again, under atmospheric environment, adopt single roller chilling band to equip and be prepared into amorphous alloy ribbon.Strip width 10mm, thickness of strip 30 μm, toughness is good, to constantly curved.Amorphous thin ribbon is wound into the magnetic core being of a size of 13.2 × 21.5 × 10 mm.Finally in vacuum annealing furnace, carry out isothermal annealing Crystallizing treatment, optimum treatment process is: 480 degree of preannealings 60 minutes, 550 DEG C of subsequent annealings 90 minutes, are quickly cooled to less than 350 DEG C to come out of the stove then to carry out air-cooled to room temperature, obtained magnetic core initial permeability μ at 50 hz after heat treatment
0(during H=0.04A/m) is greater than 140,000 Gs/Oe, during saturation induction density B(H=5A/m) be greater than 1.0T.
Embodiment 5
The chemical composition of foundry alloy is: Fe 83.37, Si 7.70, B 1.98, Cu 1.29, Nb 5.66(wt%).First the melting under atmospheric environment of Frequency Induction Heating smelting furnace is adopted to prepare foundry alloy.Secondly foundry alloy carries out remelting under the protection of steel-making slag former, and removes clean before system band.Again, under atmospheric environment, adopt single roller chilling band to equip and be prepared into amorphous alloy ribbon.Strip width 10mm, thickness of strip 30 μm, toughness is good, to constantly curved.Amorphous thin ribbon is wound into the magnetic core being of a size of 13.2 × 21.5 × 10 mm.Finally in vacuum annealing furnace, carry out isothermal annealing Crystallizing treatment, optimum treatment process is: 480 degree of preannealings 60 minutes, 550 DEG C of subsequent annealings 90 minutes, be quickly cooled to less than 350 DEG C to come out of the stove after heat treatment then to carry out air-cooled to room temperature, during the effective permeability μ e(H=0.05A/m of obtained magnetic core under 1kHz condition) be greater than 100,000 Gs/Oe, loss P under 20kHz, 0.2T condition
0.2/20k=5.6 W/kg.
Claims (10)
1. an iron-based amorphous and nanocrystalline soft magnetic alloy, it is characterized in that, be the FeSiBCuNb alloy be made up of iron, silicon, boron, copper, niobium, wherein the mass percent of each chemical composition is respectively Si7 ~ 10%, B1.8 ~ 2.2%, Cu1 ~ 1.5%, Nb4 ~ 6%, surplus be Fe.
2. as claim 1 so iron-based amorphous and nanocrystalline soft magnetic alloy, it is characterized in that, the mass percent of described Nb is 4 ~ 5.66%.
3. a preparation method for iron-based amorphous and nanocrystalline soft magnetic alloy, is characterized in that, the method comprises the following steps:
(1) proportioning foundry alloy raw material: by the according to chemical composition mass percent configuration of Armco iron, Commercial multicrystalline silicon, industrial ferro-boron, industrial ferro-niobium, cathode copper, wherein Si 7 ~ 10%; B 1.8 ~ 2.2%; Cu 1.0 ~ 1.5%; Nb 4 ~ 6%; Its surplus is Fe;
(2) foundry alloy melting: 1. foundry alloy raw material good for proportioning is positioned over mid-frequency melting furnace in top by the order of a small amount of Armco iron and industrial ferro-niobium, a small amount of industrial ferro-boron and a small amount of Armco iron, cathode copper, surplus industry ferro-boron and a small amount of Armco iron, Commercial multicrystalline silicon, surplus Armco iron from bottom smelting furnace, keeps mid-frequency melting furnace initial power 20-40kW;
2. when step 1. in foundry alloy material temperature reach 300-380 spend time, power rises to 80-100kW;
3. when step 2. in bottom smelting furnace the temperature of foundry alloy raw material reach 1100-1535 spend time, foundry alloy raw material starts to melt and foundry alloy raw material integral sinking, and mid-frequency melting furnace power rises to 140-160kW;
4. when 3. middle foundry alloy raw material melts step completely, stop heating, steelmaking slag agent be covered in anti-oxidation on alloy molten solution and remove the gred, keeping after 5-10 minute, slag former is removed clean;
5. by the mid-frequency melting furnace inclination 15-20 ° after step 4. melting, and regulate mid-frequency melting furnace power to 30-40kW, keep 1-2 minute, rapidly power is risen to 100-120kW, alloy molten solution is rolled in smelting furnace, keep again power being down to 30-40kW after 3-5 minute, repeat this step 3-5 time;
6. after 5. step has operated, stop heating, alloy molten solution steelmaking slag agent covers anti-oxidation and removes the gred, retention time 5-10 minute, is removed by slag former clean, and after repeating 3-5 time, alloy molten solution casting is come out of the stove, obtained master alloy ingot;
(3) amorphous thin ribbon is prepared: the master alloy ingot first step (2) prepared is broken, add the Frequency Induction Heating melting refusion in the stove of pocket builder, in process, alloy molten solution steelmaking slag agent covers anti-oxidation, remove clean before system band, then, under atmospheric environment, adopt single roller chilling band method that the alloy molten solution of remelting is prepared into amorphous thin ribbon;
(4) nano-crystallization process: the amorphous thin ribbon that step (3) obtains is put into vacuum annealing furnace and carries out isothermal annealing Crystallizing treatment, obtains containing Si 7 ~ 10%; B 1.8 ~ 2.2%; Cu1.0 ~ 1.5%; Nb 4 ~ 6%; Surplus is the iron-based amorphous and nanocrystalline soft magnetic alloy of Fe.
4. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as described in claim 3, it is characterized in that, in described foundry alloy raw material, each chemical composition mass percent is respectively Si 7 ~ 10%; B 1.8 ~ 2.2%; Cu 1.0 ~ 1.5%; Nb 4 ~ 5.66%; Surplus is Fe.
5. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as claimed in claim 3, it is characterized in that, in described foundry alloy, each chemical composition mass percent is: Si 9.56%, B 1.94%, Cu 1.38%, Nb 5.37%, and surplus is Fe.
6. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as claimed in claim 3, it is characterized in that, in described foundry alloy, each chemical composition mass percent is: Si 9.25%, B 1.94%, Cu 1.37%, Nb 5.26%, and surplus is Fe.
7. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as claimed in claim 3, it is characterized in that, in described foundry alloy, each chemical composition mass percent is: Si 9.56%, B 1.94%, Cu 1.38%, Nb 5.46%, and surplus is Fe.
8. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as claimed in claim 3, it is characterized in that, in described foundry alloy, each chemical composition mass percent is: Si 7.70%, B 1.98%, Cu 1.29%, Nb 5.66%, and surplus is Fe.
9. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as claimed in claim 3, it is characterized in that, in described foundry alloy, each chemical composition mass percent is: Si 9.246%, B 1.935%, Cu 1.373%, Nb 5.352%, and surplus is Fe.
10. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as described in as arbitrary in claim 3 to 9, it is characterized in that, described isothermal annealing Crystallizing treatment technique of carrying out in vacuum annealing furnace is: 480-500 degree preannealing 60 minutes, 500-550 DEG C of subsequent annealing 90 minutes, is quickly cooled to less than 350 DEG C to come out of the stove then to carry out air-cooled to room temperature after heat treatment.
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| CN107424707A (en) * | 2017-08-11 | 2017-12-01 | 南京信息工程大学 | A kind of soft magnetic materials and preparation method thereof |
| CN108559926A (en) * | 2018-01-30 | 2018-09-21 | 江苏奥玛德新材料科技有限公司 | A kind of preparation method of Fe-based amorphous band and preparation method thereof and high frequency high magnetic permeability nanometer crystal alloy |
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| CN107309408A (en) * | 2017-06-28 | 2017-11-03 | 黄毅 | The method of the high permeability amorphous nanocrystalline alloy band of low cost production |
| CN107309408B (en) * | 2017-06-28 | 2019-04-05 | 黄毅 | The method that low cost produces high permeability amorphous nanocrystalline alloy band |
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| CN113539653A (en) * | 2021-09-16 | 2021-10-22 | 西安钢研功能材料股份有限公司 | Preparation method of high-strength soft magnetic alloy bar |
| CN114045435A (en) * | 2021-11-11 | 2022-02-15 | 泉州天智合金材料科技有限公司 | Iron-based amorphous nanocrystalline wave-absorbing material and preparation method thereof |
| CN114672742A (en) * | 2022-03-02 | 2022-06-28 | 宁波辰磁电子科技有限公司 | Nanocrystalline alloy magnetic core and preparation method thereof |
| CN114672742B (en) * | 2022-03-02 | 2023-02-28 | 宁波辰磁电子科技有限公司 | Nanocrystalline alloy magnetic core and preparation method thereof |
| CN114959213A (en) * | 2022-04-13 | 2022-08-30 | 宁波中科毕普拉斯新材料科技有限公司 | Heat treatment method of high-frequency low-loss iron-based nanocrystalline magnetic core |
| CN115161449A (en) * | 2022-07-18 | 2022-10-11 | 华中科技大学 | Heat treatment method of amorphous alloy |
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