CN113035485A - High-magnetic-flux-density low-loss iron-based nanocrystalline magnetically soft alloy and preparation method thereof - Google Patents

High-magnetic-flux-density low-loss iron-based nanocrystalline magnetically soft alloy and preparation method thereof Download PDF

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CN113035485A
CN113035485A CN202110239629.1A CN202110239629A CN113035485A CN 113035485 A CN113035485 A CN 113035485A CN 202110239629 A CN202110239629 A CN 202110239629A CN 113035485 A CN113035485 A CN 113035485A
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耿振伟
胡庚
朱圆圆
韩仕杰
王雪珂
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Shenzhen Microgate Technology Co ltd
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Abstract

The invention discloses a high-flux-density low-loss iron-based nanocrystalline soft magnetic alloy and a preparation method thereof, aiming at meeting the requirements of miniaturization and high power of magnetic components such as high-frequency inductors, high-frequency switching power supplies, high-frequency transformers and the like, the invention discloses the high-flux-density low-loss iron-based nanocrystalline soft magnetic alloy and the preparation method thereof, wherein the composition of the high-flux-density low-loss iron-based nanocrystalline soft magnetic alloy meets the following molecular formula: FeaCobWcBdSieCufAlgMi, wherein M is one of C, P, Cr, Ti or Mn, subscripts a, b, C, d, e, f, g and i are respectively the atom percentage content of corresponding elements, and satisfy the conditions that a is more than or equal to 10.0 and less than or equal to 85.0, b is more than or equal to 10.0 and less than or equal to 85.0, C is more than or equal to 2.0 and less than or equal to 4.5, d is more than or equal to 3.5 and less than or equal to 18.5, e is more than or equal to 1.5 and less than or equal to 10.0, f is more than or equal to 0.3 and less than or equal to 1.2, g is more than or equal to 0.5 and less than or equal to 2.5, g is more than or equal to 0.5 and less than or equal to 6; the nanocrystalline magnetically soft alloy prepared by the method has the beneficial effects of high magnetic flux density, low loss and high magnetic conductivity.

Description

High-magnetic-flux-density low-loss iron-based nanocrystalline magnetically soft alloy and preparation method thereof
Technical Field
The invention belongs to the field of iron-based nanocrystalline magnetically soft alloys, and relates to a preparation method of an iron-based nanocrystalline magnetically soft alloy with high magnetic flux density and low loss.
Background
With the progress of technology, in order to achieve miniaturization and high efficiency of electronic components such as transformers and inductors, a soft magnetic composite material is generally required to have a higher magnetic flux density and a lower loss. The soft magnetic composite material is composed of soft magnetic powder and a binder, wherein the magnetic powder has a main influence on the magnetic flux density and the loss of the soft magnetic composite material. The soft magnetic powder comprises pure iron soft magnetic powder, ferrosilicon soft magnetic powder, ferronickel soft magnetic powder, soft magnetic ferrite, amorphous soft magnetic powder, nanocrystalline soft magnetic powder and the like, wherein the amorphous soft magnetic powder and the nanocrystalline soft magnetic powder are widely applied to the market with the advantage of excellent low loss performance in recent years, and the nanocrystalline soft magnetic powder is prepared from the amorphous soft magnetic powder by heat treatment annealing, mainly comprises an amorphous matrix and nanocrystalline grains and has the characteristics of the traditional crystalline soft magnetic material and the amorphous soft magnetic material.
The Fe-based nanocrystalline magnetically soft alloy which is commonly used at present is mainly a FINMET alloy, the main component of the Fe-Si-B-M-Cu nanocrystalline alloy has the characteristics of high magnetic conductivity, low loss and the like, but the saturation magnetic induction intensity of the nanocrystalline alloy is lower, wherein Fe is used73.6Nb3Si13.5B9Cu1Typically, the saturation magnetic induction is only 1.24T, and the application is limited.
In order to meet the requirements of development of modern military and civil industries and the requirements of miniaturization and high power of magnetic components such as high-frequency inductors, high-frequency switching power supplies, high-frequency transformers and the like, the development of an iron-based nanocrystalline magnetically soft alloy material with high magnetic flux density and low loss is urgently needed
Disclosure of Invention
The invention discloses a high-flux density low-loss iron-based nanocrystalline soft magnetic alloy and a preparation method thereof, wherein the composition of the high-flux density low-loss iron-based nanocrystalline soft magnetic alloy meets the following molecular formula: feaCobWcBdSieCufAlgMiWherein M is one of C, P, Cr, Ti or Mn, subscripts a, b, C, d, e, f, g and i are atom percentage contents of corresponding elements respectively, and satisfy that a is not less than 10.0 and not more than 85.0, b is not less than 10.0 and not more than 85.0, C is not less than 2.0 and not more than 4.5, d is not less than 3.5 and not more than 18.5, e is not less than 1.5 and not more than 10.0, f is not less than 0.3 and not more than 1.2, g is not less than 0.5 and not more than 2.5, g is not less than 0.5 and not more than 8.5, i is not less than 0.5 and not more than 6.0, and a + b + C + d + e + f + g + i is 100, so that the nano-crystal softThe nanocrystalline soft magnetic powder mainly comprises elements such as Fe, Co, W, B, Si, Cu, Al and the like, wherein the addition of the Co element mainly improves the magnetic flux density Bs and the Curie temperature Tc of the nanocrystalline soft magnetic powder, the addition of the W, B, Si and Al mainly improves the amorphous nuclear capacity of the nanocrystalline soft magnetic powder, and the addition of the Cu element mainly improves the nanocrystalline nuclear capacity of the nanocrystalline soft magnetic powder in the heat treatment process.
The invention also provides a preparation method of the iron-based nanocrystalline magnetically soft alloy with high magnetic flux density and low loss, which comprises the following steps:
1) preparing materials: weighing each element raw material with the mass percentage purity not lower than 99% according to the molecular formula, and blending;
2) smelting a master alloy: adding the raw materials prepared in the step 1) into a crucible of a smelting furnace, smelting alloy raw materials, and uniformly removing slag to obtain a master alloy ingot, wherein the smelting temperature is 1350-;
3) atomizing to prepare powder: remelting the master alloy ingot prepared in the step 2) on atomization powder making equipment, and atomizing to prepare the iron-based amorphous magnetically soft alloy after the master alloy is completely molten;
4) and (3) heat treatment: putting the iron-based amorphous magnetically soft alloy powder prepared in the step 3) into a heat treatment equipment furnace for heat treatment to separate out nanocrystalline grains, and taking out the nanocrystalline magnetically soft alloy material after heat treatment, wherein the heat treatment temperature is 450-550 ℃.
The nanocrystalline magnetically soft alloy prepared by the method has the beneficial effects of high magnetic flux density, low loss and high magnetic conductivity.
Drawings
FIG. 1 is an XRD representation of the atomized powder of the Fe-based amorphous soft magnetic alloy in example 1;
FIG. 2 is a XRD representation of the heat treatment of the Fe-based amorphous soft magnetic alloy of example 1;
fig. 3 is an SEM picture of the nanocrystalline soft magnetic alloy prepared in example 1.
Detailed Description
Example 1
In example 1, the molecular formula of the iron-based nanocrystalline magnetically soft alloy is Fe65Co15W2B10Si2.5Cu1Al0.5Ti4。
1) The raw materials of each element with the purity of not less than 99 percent are mixed according to the molecular formula
Fe65Co15W2B10Si2.5Cu1Al0.5Ti4And (4) batching according to atomic percentage.
2) The ingredients in the step 1) are loaded into an electric arc melting furnace, and the electric arc melting is carried out for 3 times so as to ensure that the components of the master alloy are uniform, and the melting temperature is 1900 ℃.
3) Putting the master alloy obtained in the step 2) into an atomizing equipment smelting furnace, and carrying out water-gas combined atomization to prepare amorphous magnetically soft alloy powder. Carrying out XRD characterization on the iron-based amorphous soft magnetic alloy, as shown in figure 1; the materialization preparation method is water-gas combined atomization powder preparation.
4) And carrying out heat treatment on the amorphous magnetically soft alloy powder, keeping the temperature at 500 ℃ for 30 minutes, and carrying out air cooling after the heat treatment is finished to obtain the nanocrystalline magnetically soft alloy powder. The iron-based nanocrystalline magnetically soft alloy is subjected to XRD characterization, as shown in figure 2.
5) Adding 1.0-6.0% of binder into the nanocrystalline magnetically soft alloy powder prepared in the step 4), pressing the mixture under 500MP to form a ring with OD ID H-20H-6H-1.5-2.0 mm, and curing the ring for 2 hours at the temperature of 180 ℃.
Example 2
In this example 2, the molecular formula of the iron-based nanocrystalline magnetically soft alloy is Fe60Co25W1B8Si2.5Cu1Al0.5Ti2。
1) Using raw materials of elements with purity not lower than 99% according to the molecular formula Fe60Co25W1B8Si2.5Cu1Al0.5Ti2And (4) batching according to atomic percentage.
2) And (3) putting the ingredients in the step 5) into an electric arc melting furnace, and carrying out electric arc melting for 3 times to ensure that the components of the master alloy are uniform, wherein the melting temperature is 1900 ℃.
3) Putting the master alloy obtained in the step 6) into an atomizing equipment smelting furnace, and carrying out water-gas combined atomization to prepare amorphous magnetically soft alloy powder.
4) And carrying out heat treatment on the amorphous magnetically soft alloy powder, keeping the temperature at 500 ℃ for 30 minutes, and carrying out air cooling after the heat treatment is finished to obtain the nanocrystalline magnetically soft alloy powder.
Adding 1.0-6.0% of binder into the nanocrystalline magnetically soft alloy powder prepared in the step 8), pressing the mixture under 500MP to form a ring with OD ID H-20H-6H-1.5-2.0 mm, and curing the ring for 2 hours at the temperature of 180 ℃.
Comparative examples
In the comparative example of the embodiment, the molecular formula of the iron-based nanocrystalline magnetically soft alloy is Fe73.6Nb3Si13.5Cu1B9。
1) Using raw materials of elements with purity not lower than 99% according to the molecular formula Fe73.6Nb3Si13.5Cu1B9And (4) batching according to atomic percentage.
2) The ingredients in the step 1) are loaded into an electric arc melting furnace, and the electric arc melting is carried out for 3 times so as to ensure that the components of the master alloy are uniform, and the melting temperature is 1600 ℃.
3) Putting the master alloy obtained in the step 2) into an atomizing equipment smelting furnace, and carrying out water-gas combined atomization to prepare amorphous magnetically soft alloy powder.
4) And carrying out heat treatment on the amorphous magnetically soft alloy powder, keeping the temperature at 500 ℃ for 30 minutes, and carrying out air cooling after the heat treatment is finished to obtain the nanocrystalline magnetically soft alloy powder.
Adding 1.0-6.0% of binder into the nanocrystalline magnetically soft alloy powder prepared in the step 4), pressing the mixture under 500MP to form a ring with OD ID H-20H-6H-1.5-2.0 mm, and curing the ring for 2 hours at the temperature of 180 ℃.
The performance tests were performed on the nanocrystalline soft magnetic alloy powders in the examples and comparative examples, and the data are as follows:
Figure BDA0002961669030000051

Claims (3)

1. heightThe magnetic flux density low-loss iron-based nanocrystalline soft magnetic alloy is characterized in that the composition of the high magnetic flux density low-loss iron-based nanocrystalline soft magnetic alloy meets the following molecular formula: feaCobWcBdSieCufAlgMiWherein M is one of C, P, Cr, Ti or Mn, subscripts a, b, C, d, e, f, g and i are the atom percentage contents of the corresponding elements respectively, and satisfy that a is more than or equal to 10.0 and less than or equal to 85.0, b is more than or equal to 10.0 and less than or equal to 85.0, C is more than or equal to 2.0 and less than or equal to 4.5, d is more than or equal to 3.5 and less than or equal to 18.5, e is more than or equal to 1.5 and less than or equal to 10.0, f is more than or equal to 0.3 and less than or equal to 1.2, g is more than or equal to 0.5 and less than or equal to 2.5, g is more than or equal to 0.5 and less than or equal to 8.5.
2. A preparation method of a high-magnetic flux density low-loss iron-based nanocrystalline magnetically soft alloy is characterized by comprising the following steps:
1) preparing materials: weighing each element raw material with the mass percent purity of not less than 99 percent according to the molecular formula of claim 1, and blending;
2) smelting a master alloy: adding the raw materials prepared in the step 1) into a crucible of a smelting furnace, smelting alloy raw materials, and uniformly removing slag to obtain a master alloy ingot, wherein the smelting temperature is 1350-;
3) atomizing to prepare powder: remelting the master alloy ingot prepared in the step 2) on atomization powder making equipment, and atomizing to prepare the iron-based amorphous magnetically soft alloy after the master alloy is completely molten;
4) and (3) heat treatment: putting the iron-based amorphous magnetically soft alloy powder prepared in the step 3) into a heat treatment equipment furnace for heat treatment; after heat treatment, taking out to obtain the nanocrystalline soft magnetic alloy material, wherein the heat treatment temperature is 450-550 ℃.
3. The method of claim 2, wherein the atomization in step 2) is a water-gas combined atomization process.
CN202110239629.1A 2021-03-04 2021-03-04 High-magnetic-flux-density low-loss iron-based nanocrystalline magnetically soft alloy and preparation method thereof Pending CN113035485A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115608996A (en) * 2021-07-28 2023-01-17 中国科学院宁波材料技术与工程研究所 Iron-based nanocrystalline magnetically soft alloy powder and preparation method thereof
CN115608996B (en) * 2021-07-28 2024-05-03 中国科学院宁波材料技术与工程研究所 Iron-based nanocrystalline magnetically soft alloy powder and preparation method thereof

Citations (3)

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Publication number Priority date Publication date Assignee Title
US20100097171A1 (en) * 2007-03-20 2010-04-22 Akiri Urata Soft magnetic alloy, magnetic component using the same, and thier production methods
CN102543348A (en) * 2012-01-09 2012-07-04 上海米创电器有限公司 Iron-based nanocrystalline magnetically soft alloy and preparation method thereof
CN102719746A (en) * 2012-07-02 2012-10-10 苏州宝越新材料科技有限公司 Iron-based nanocrystalline magnetically soft alloy material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100097171A1 (en) * 2007-03-20 2010-04-22 Akiri Urata Soft magnetic alloy, magnetic component using the same, and thier production methods
CN102543348A (en) * 2012-01-09 2012-07-04 上海米创电器有限公司 Iron-based nanocrystalline magnetically soft alloy and preparation method thereof
CN102719746A (en) * 2012-07-02 2012-10-10 苏州宝越新材料科技有限公司 Iron-based nanocrystalline magnetically soft alloy material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115608996A (en) * 2021-07-28 2023-01-17 中国科学院宁波材料技术与工程研究所 Iron-based nanocrystalline magnetically soft alloy powder and preparation method thereof
CN115608996B (en) * 2021-07-28 2024-05-03 中国科学院宁波材料技术与工程研究所 Iron-based nanocrystalline magnetically soft alloy powder and preparation method thereof

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