CN104485192B - A kind of iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof - Google Patents
A kind of iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof.First the mass percent of the most each chemical composition of proportioning foundry alloy raw material is respectively Si7 ~ 10%, B1.8 ~ 2.2%, Cu1 ~ 1.5%, Nb4 ~ 6%, surplus are Fe；By foundry alloy raw material melt back and pour into alloy pig；By broken for alloy pig and melting again, and cover with steelmaking slag agent；Single roller chilling band method is used to prepare amorphous thin ribbon；The amorphous thin ribbon obtained is put in vacuum annealing furnace and carry out isothermal annealing Crystallizing treatment；Then cool to room temperature with the furnace, obtain iron-based amorphous and nanocrystalline soft magnetic alloy.Raw material used in the present invention is the raw material of industry of low cost, coordinates the preparation method of the present invention so that the iron-based amorphous and nanocrystalline soft magnetic alloy of the present invention has low cost, the characteristic of high magnetic permeability.
Description
Technical field
The present invention is belonging to magnetic material and preparing technical field thereof, especially relates to a kind of low-loss Fe-based nanocrystalline magnetically soft alloy of high permeability and preparation method thereof.
Background technology
Along with social development, in fields such as power system, computer network, multimedia technology and high frequency micro-magnetic device, increasingly require components and parts high-quality, small-sized, light weight used, this just requires that the Metallic Functional Materials such as used magnetically soft alloy improve constantly performance, i.e. this soft magnetic materials to have both high saturation and magnetic intensity (Bs) and high permeability (μ) simultaneously.The breakthrough being the discovery that this difficult problem of solution of " Finemet " nano-crystal soft magnetic alloy.This magnetically soft alloy has high saturation and magnetic intensity (Bs: 1.24T), high initial magnetic permeability (μ0 : 8 x 104Gs/Oe), low iron loss (Ps0.5/20k : 20W/kg) etc. characteristic, be widely used.
The Exemplary chemical composition of " Finemet " nano-crystal soft magnetic alloy is Fe73.5Cu1Nb3Si13.5B9, its preparation principle is first to be prepared amorphous alloy strips by fast solidification technology, forms amorphous and Nanocrystalline Two-phase structure after being then passed through suitable temperature subsequent annealing, and wherein Cu segregation separates out in advance, at Cu cluster periphery α-FeSi
Carrying out forming core again, therefore Cu has the effect promoting forming core；And Nb discharges from α-FeSi crystal grain, it is enriched with in residue amorphous phase, and stably remains 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 typically larger than 5%, but Nb's is expensive, Nb element occupies more than the 70% of raw material totle drilling cost, and this causes the cost of raw material of iron-base nanometer crystal alloy the highest, is unfavorable for industrialized production.
Chinese invention patent CN 1621550A discloses a kind of Fe76.5-x-y-zCu1NbxVySizB9(atomic ratio) Fe-based nanocrystalline magnetically soft alloy, and 0 < X < 5,0 < Y < 7,0 < Z < 20, use V part to instead of Nb.This invention Fe-based nanocrystalline magnetically soft alloy can process without magnetic field and has special squareness ratio and can reduce the cost of raw material, but, relative Fe73.5Si13.5B9Cu1Nb3For nano-crystal soft magnetic alloy, the permeability of such Fe-based nanocrystalline magnetically soft alloy declines, and coercivity rises.
Open CN 103187136 A of Chinese invention patent discloses a kind of Fe-based amorphous soft magnetic materials, and this material is FeaYbSicBd(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.Have an advantage in that: FeaYbSicBdThe non-crystaline amorphous metal of system has bigger amorphous formation ability, excellent saturation induction density, low-coercivity and high initial permeability.It is Fe that described material preferably constitutes chemical composition77Y1Si9B13And Fe76Y2Si9B13(atomic ratio), its saturation induction density is respectively 1.67 T and 1.60 T, but, the parameter such as the coercivity of this material, permeability and loss is not mentioned.Further, due to the addition of oxidizable Rare Earth Y so that complicated process of preparation, it is unfavorable 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 characterised in that it is the Fe being made up of iron, silicon, boron, phosphorus, copperxSiyBzPaCubAlloy, in formula, x, y, z, a, b represent the atom percentage content of each corresponding component, wherein x=70-90%, y=1-15%, z=1-20%, a=1-20%, b=0.1-1%, and x+y+z+a+b=100% respectively；The micro-structural of this Fe-based nanocrystalline magnetically soft alloy is the size body-centered cubic α-Fe(Si between 1-35nm) nanometer crystalline phase coexists with the amorphous phase rich in phosphorus and boron, and with amorphous phase for matrix phase.Raw material good for proportioning is mainly first prepared as 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 can be greatly improved the saturation magnetization of nano-crystal soft magnetic alloy, can keep relatively low coercivity and effectively reduce the cost of raw material simultaneously.But the interpolation of P can cause alloy easily to aoxidize in preparation process, collapse and spatter, alloying component is wayward, is unfavorable for industrialized production, and gained nano crystal soft magnetic material is relative to Fe73.5Si13.5B9Cu1Nb3For nanometer crystal alloy, coercivity rises.
Summary of the invention
The invention aims to overcome the deficiency of above-mentioned existing existence to provide high permeability low-loss iron-based amorphous and nanocrystalline soft magnetic alloy of a kind of high-performance, low cost and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions: according to the purpose of the present invention, we are to be suitable for industrial mass production by the iron-based amorphous and nanocrystalline soft magnetic alloy FeSiBCuNb purpose designed by optimization of Chemical Composition, should possess the features such as ratio iron-based amorphous and nanocrystalline soft magnetic alloy lower cost of the prior art, higher permeability and lower loss.Raw material used in the present invention is the raw material of industry of low cost, prior art uses the raw material of the present invention cannot prepare 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 characterised 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 the preferably Nb content in industrial iron-based amorphous and nanocrystalline soft magnetic alloy material composition of one in the present invention is less than 5.66%.
The present invention also provides for a kind of method of iron-based amorphous and nanocrystalline soft magnetic alloy aiming at and manufacturing the present invention, and the method comprises the following steps:
(1) proportioning foundry alloy raw material: raw material all use the existing industrial raw material being easier to start with and price is less expensive, such as ingot iron, Commercial multicrystalline silicon, industry ferro-boron, industry ferro-niobium, cathode copper.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 in mid-frequency melting furnace by a small amount of ingot iron-industry ferro-niobium, a small amount of industry ferro-boron-a small amount of ingot iron, cathode copper, surplus industry ferro-boron-a small amount of ingot iron, Commercial multicrystalline silicon, the order of surplus ingot iron to top 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 step 3. in foundry alloy raw material be completely melt time, stop heating, steelmaking slag agent be covered on alloy molten solution anti-oxidation and remove the gred, after keeping 5-10 minute, slag former is removed totally；
5. the alloy solution after step 4. melting is turned forward 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 made to roll in smelting furnace, again power is down to 30-40kW after keeping 3-5 minute, repeats this step 3-5 time；
6. after 5. step has operated, stopping heating, alloy molten solution steelmaking slag agent covers anti-oxidation and removes the gred, 5-10 minute retention time, is removed by slag former clean, and after repeating 3-5 time, alloy molten solution casting is come out of the stove, and prepares master alloy ingot；
(3) amorphous thin ribbon is prepared: the master alloy ingot first step (2) prepared crushes, add the Frequency Induction Heating melting refusion in the stove of pocket builder, during alloy molten solution steelmaking slag agent cover anti-oxidation, remove clean before system band, then, under atmospheric environment, use single roller chilling band method that the alloy molten solution of remelting is prepared as amorphous thin ribbon；
(4) nano-crystallization processes: is put into by the amorphous thin ribbon that step (3) obtains and carries out isothermal annealing Crystallizing treatment in vacuum annealing furnace；
Preferred strip width 10mm of Fe-based amorphous nanocrystalline alloy prepared by the present invention, thickness of strip 30 μm.
The process of preferred steps (4) nano-crystallization carries out isothermal annealing Crystallizing treatment technique in vacuum annealing furnace and is: 480-500 degree preannealing 60 minutes, 500-550 DEG C of subsequent annealing 90 minutes, be quickly cooled to after heat treatment less than 350 DEG C come out of the stove then carry out air-cooled to room temperature.
A kind of iron-based amorphous and nanocrystalline soft magnetic alloy in the present invention be carry out on the basis of traditional soft magnetic alloy optimizing components have chosen Fe, Si, B, Cu, Nb five elements, and the content reducing Nb realize reduce material cost；It addition, the raw material required for preparing foundry alloy in the present invention all use industrial raw material, the method with the use of the present invention prepares iron base amorphous magnetically-soft alloy, reduces material cost, more conducively industrial mass production simultaneously.Further, low cost, high permeability and low-loss iron-based amorphous and nanocrystalline soft magnetic alloy are prepared.
Detailed description of the invention
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%).Foundry alloy is prepared initially with the melting under atmospheric environment of Frequency Induction Heating smelting furnace.Secondly foundry alloy carries out remelting under steel-making slag former is protected, and removes clean before system band.Again, under atmospheric environment, single roller chilling band equipment is used to be prepared as amorphous alloy ribbon.Strip width 10mm, thickness of strip 30 μm, toughness is good, to curved constantly.Amorphous thin ribbon is wound into the magnetic core 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 after heat treatment less than 350 DEG C come out of the stove then carry out air-cooled to room temperature, during obtained magnetic core effective permeability μ e(H=0.05A/m under the conditions of 1kHz) more than 140,000 Gs/Oe, loss P under the conditions of 20kHz, 0.2T0.2/20k = 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%).Foundry alloy is prepared initially with the melting under atmospheric environment of Frequency Induction Heating smelting furnace.Secondly foundry alloy carries out remelting under steel-making slag former is protected, and removes clean before system band.Again, under atmospheric environment, single roller chilling band equipment is used to be prepared as amorphous alloy ribbon.Strip width 10mm, thickness of strip 30 μm, toughness is good, to curved constantly.Amorphous thin ribbon is wound into the magnetic core 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 after heat treatment less than 350 DEG C come out of the stove then carry out air-cooled to room temperature, during obtained magnetic core effective permeability μ e(H=0.05A/m under the conditions of 1kHz) more than 120,000 Gs/Oe, loss P under the conditions of 20kHz, 0.2T0.2/20k = 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%).Foundry alloy is prepared initially with the melting under atmospheric environment of Frequency Induction Heating smelting furnace.Secondly foundry alloy carries out remelting under steel-making slag former is protected, and removes clean before system band.Again, under atmospheric environment, single roller chilling band equipment is used to be prepared as amorphous alloy ribbon.Strip width 10mm, thickness of strip 30 μm, toughness is good, to curved constantly.Amorphous thin ribbon is wound into the magnetic core 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 after heat treatment less than 350 DEG C come out of the stove then carry out air-cooled to room temperature, during obtained magnetic core effective permeability μ e(H=0.05A/m under the conditions of 1kHz) more than 130,000 Gs/Oe, loss P under the conditions of 20kHz, 0.2T0.2/20k = 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%).Foundry alloy is prepared initially with the melting under atmospheric environment of Frequency Induction Heating smelting furnace.Secondly foundry alloy carries out remelting under steel-making slag former is protected, and removes clean before system band.Again, under atmospheric environment, single roller chilling band equipment is used to be prepared as amorphous alloy ribbon.Strip width 10mm, thickness of strip 30 μm, toughness is good, to curved constantly.Amorphous thin ribbon is wound into the magnetic core 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 after heat treatment less than 350 DEG C come out of the stove then carry out air-cooled to room temperature, obtained magnetic core initial permeability μ at 50 hz0(during H=0.04A/m) is more than 140,000 Gs/Oe, during saturation induction density B(H=5A/m) more 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%).Foundry alloy is prepared initially with the melting under atmospheric environment of Frequency Induction Heating smelting furnace.Secondly foundry alloy carries out remelting under steel-making slag former is protected, and removes clean before system band.Again, under atmospheric environment, single roller chilling band equipment is used to be prepared as amorphous alloy ribbon.Strip width 10mm, thickness of strip 30 μm, toughness is good, to curved constantly.Amorphous thin ribbon is wound into the magnetic core 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 after heat treatment less than 350 DEG C come out of the stove then carry out air-cooled to room temperature, during obtained magnetic core effective permeability μ e(H=0.05A/m under the conditions of 1kHz) more than 100,000 Gs/Oe, loss P under the conditions of 20kHz, 0.2T0.2/20k = 5.6
W/kg。
Claims (8)
1. the preparation method of an iron-based amorphous and nanocrystalline soft magnetic alloy, it is characterized in that, described iron-based amorphous and nanocrystalline soft magnetic alloy is the FeSiBCuNb alloy being made up of iron, silicon, boron, copper, niobium, and the mass percent of the most each chemical composition is respectively Si7 ~ 10%, B1.8 ~ 2.2%, Cu1 ~ 1.5%, Nb4 ~ 6%, surplus are Fe；Its preparation method comprises the following steps:
(1) proportioning foundry alloy raw material: by ingot iron, Commercial multicrystalline silicon, industry ferro-boron, industry ferro-niobium, cathode copper according to chemical composition mass percent configuration, 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 in mid-frequency melting furnace by a small amount of ingot iron and industry ferro-niobium, a small amount of industry ferro-boron and a small amount of ingot iron, cathode copper, surplus industry ferro-boron and a small amount of ingot iron, Commercial multicrystalline silicon, the order of surplus ingot iron to top 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 step 3. in foundry alloy raw material be completely melt time, stop heating, steelmaking slag agent be covered on alloy molten solution anti-oxidation and remove the gred, after keeping 5-10 minute, slag former is removed totally；
5. the mid-frequency melting furnace after step 4. melting is tilted 15-20 °, and regulate mid-frequency melting furnace power to 30-40kW, keep 1-2 minute, rapidly power is risen to 100-120kW, make alloy molten solution roll in smelting furnace, again power is down to 30-40kW after keeping 3-5 minute, repeats this step 3-5 time；
6. after 5. step has operated, stopping heating, alloy molten solution steelmaking slag agent covers anti-oxidation and removes the gred, 5-10 minute retention time, is removed by slag former clean, and after repeating 3-5 time, alloy molten solution casting is come out of the stove, and prepares master alloy ingot；
(3) amorphous thin ribbon is prepared: the master alloy ingot first step (2) prepared crushes, add the Frequency Induction Heating melting refusion in the stove of pocket builder, during alloy molten solution steelmaking slag agent cover anti-oxidation, remove clean before system band, then, under atmospheric environment, use single roller chilling band method that the alloy molten solution of remelting is prepared as amorphous thin ribbon；
(4) nano-crystallization processes: is put into by the amorphous thin ribbon that step (3) obtains and carries out isothermal annealing Crystallizing treatment in vacuum annealing furnace, 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.
2. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as described in claim 1, it is characterised 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.
3. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as claimed in claim 1, it is characterised 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.
4. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as claimed in claim 1, it is characterised 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.
5. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as claimed in claim 1, it is characterised 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.
6. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as claimed in claim 1, it is characterised 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.
7. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as claimed in claim 1, it is characterised 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.
8. the preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy as described in claim 1 to 7 is arbitrary, it is characterized in that, the described isothermal annealing Crystallizing treatment technique that carries out in vacuum annealing furnace is: 480-500 degree preannealing 60 minutes, 500-550 DEG C of subsequent annealing 90 minutes, be quickly cooled to after heat treatment less than 350 DEG C come out of the stove then carry out air-cooled to room temperature.
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| CN113305273A (en) * | 2021-04-16 | 2021-08-27 | 青县择明朗熙电子器件有限公司 | Preparation method of high-performance and high-stability nanocrystalline soft magnetic material |
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| 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 |
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