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CN119252643A - A kind of iron-based magnetic core with constant low magnetic permeability and its preparation method - Google Patents

A kind of iron-based magnetic core with constant low magnetic permeability and its preparation method Download PDF

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Publication number
CN119252643A
CN119252643A CN202411588568.XA CN202411588568A CN119252643A CN 119252643 A CN119252643 A CN 119252643A CN 202411588568 A CN202411588568 A CN 202411588568A CN 119252643 A CN119252643 A CN 119252643A
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iron
magnetic core
magnetic
heat treatment
permeability
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CN202411588568.XA
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申家瑜
王策
徐佳
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Foshan Zhongyan Magnetoelectric Technology Co ltd
Guangdong Institute of New Materials
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Foshan Zhongyan Magnetoelectric Technology Co ltd
Guangdong Institute of New Materials
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Abstract

The invention belongs to the field of magnetic materials, and particularly discloses an iron-based magnetic core with constant low magnetic permeability, and a preparation method and application thereof. According to the invention, the iron-based amorphous magnetic core is subjected to heat treatment of a force field and heat treatment of a magnetic field at specific temperature and pressure in sequence, so that the iron-based magnetic core with low magnetic permeability can be obtained, and the iron-based magnetic core has the characteristic of less than 1500 and constant magnetic permeability at 1-100 kHz.

Description

Iron-based magnetic core with constant low magnetic permeability and preparation method thereof
Technical Field
The invention belongs to the field of magnetic materials, and particularly relates to an iron-based magnetic core with constant low magnetic permeability, and a preparation method and application thereof.
Background
The iron-based amorphous/nanocrystalline magnetically soft alloy is typically made from a master alloy by a high-speed copper roll quenching process, and the amorphous ribbon is wound into an amorphous magnetic core. The amorphous magnetic core is generally subjected to a proper heat treatment process for finely regulating and controlling the microstructure of the alloy, namely, a single magnetic alpha-Fe phase is precipitated on an amorphous matrix and is converted into an amorphous and nanocrystalline dual-phase coexisting structure to form the nanocrystalline magnetic core, and the special dual-phase nanostructure is also a main reason that the nanocrystalline magnetic core presents excellent comprehensive soft magnetic performance, so that the heat treatment process of the magnetic core has a decisive effect on obtaining the high-performance iron-based magnetic core. However, in the heat treatment process in the prior art, the obtained nanocrystalline magnetic core generally has the characteristics of high magnetic permeability and greatly reduced along with the increase of frequency, and the magnetic permeability is too high and unstable at 1-100KHz, so that the magnetic core cannot have the characteristics of constant and low magnetic permeability at low frequency, and cannot be applied to specific application scenes such as inductors, high-current power devices and the like which need to have the magnetic permeability below 1500 at 1-100KHz, and the application of the nanocrystalline magnetic core is limited.
Therefore, development of a process for manufacturing a magnetic core is needed to realize a magnetic core with a permeability of less than 1500 at 1-100 KHz.
Disclosure of Invention
In order to solve the problem that a magnetic core with low constant magnetic permeability is difficult to obtain in the prior art, the invention provides an iron-based magnetic core with constant low magnetic permeability and a preparation method thereof.
In order to achieve the above purpose, the method specifically comprises the following technical scheme:
a method for preparing an iron-based magnetic core, comprising the steps of:
(1) Heating the iron-based amorphous magnetic core to a preset temperature and simultaneously pressurizing to a preset pressure, and then cooling to below 200 ℃ to start releasing the pressure to obtain a presintered magnetic core, wherein the preset temperature is 300-425 ℃, and the preset pressure is 60-150MPa;
(2) And performing magnetic field heat treatment on the presintered magnetic core, and cooling to obtain the iron-based magnetic core.
According to the method, the iron-based amorphous magnetic core is subjected to force field heat treatment and magnetic field heat treatment at specific temperature and pressure in sequence to regulate and control the grain size, grain orientation and magnetic anisotropy, so that the iron-based magnetic core has the characteristic of effective magnetic conductivity of 100-1499 at the frequency of 1-100kHz, and the application scene of the iron-based magnetic core is widened.
Under the heat treatment of the force field, on one hand, pressure promotes the precipitation of nano crystal grains and simultaneously inhibits the rapid growth of the nano crystal grains, the magnetic core is kept at relatively low magnetic permeability and relatively stable magnetic permeability to a certain extent by controlling the crystal grain size, on the other hand, the existence of the force field can induce magnetic anisotropy in the magnetic core, the domain wall energy is improved, the high domain wall can prevent the movement of the domain wall, and the magnetic core magnetic permeability is relatively low and relatively stable by controlling the domain wall energy to a certain extent. The inventors of the present invention found that the temperature and pressure of the heat treatment of the force field have a very pronounced effect on the permeability and its stability. Under the heat treatment of a force field at 300-425 ℃, the magnetic core can still keep relatively low magnetic permeability and relatively stable magnetic permeability, but slightly deviate from the temperature range, the magnetic permeability is overlarge and the magnetic permeability stability is drastically reduced due to the high temperature, and the magnetic permeability stability is drastically reduced although the magnetic permeability meets the requirement, but the magnetic permeability stability is not met. The magnetic core can maintain relatively low magnetic permeability and relatively stable magnetic permeability under the pressure of a force field with the pressure of 60-150MPa, but the magnetic permeability of the magnetic core is slightly deviated from the pressure range, and the magnetic permeability of the magnetic core meets the requirement, but the stability of the magnetic permeability cannot meet the requirement. Therefore, the thermal field of the invention is actually a heat treatment mode of rapid heating and rapid cooling, under the synergistic effect of specific temperature and high pressure, nano crystal grains are promoted to be continuously precipitated, meanwhile, the growth of the nano crystal grains is restrained, the crystal grain state and size in a magnetic core are controlled, and meanwhile, domain wall energy is improved to a certain extent, so that the performance effects of low magnetic permeability and constant magnetic permeability of the magnetic core are realized as a whole. The actual effect of the magnetic field heat treatment is to induce grain oriented growth, i.e. to induce orientation of the nano-grains in the direction of the magnetic field application, thereby inducing magnetic anisotropy and regulating the hysteresis loop shape. The force field heat treatment and the magnetic field heat treatment are mutually matched, and the grain orientation growth is induced by the magnetic field heat treatment under the basis of regulating and controlling the grain and magnetic domain wall energy by the force field heat treatment, so that the prepared magnetic core cannot keep the performance of low-frequency low-constant magnetic permeability under the condition that the pressurization is larger than the atmospheric pressure or the condition that a constant magnetic field is added, and the performance requirement of the invention that the effective magnetic permeability is 100-1499 under the frequency of 1-100kHz cannot be realized.
Preferably, in the step (1), the iron-based amorphous magnetic core comprises the following elements in atomic percent, namely, 60-80% of Fe, 10-20% of Si, 0-10% of B, 0-3% of Cu, 0-5% of Nb, 0-15% of Ni and 0-10% of Co.
Further preferably, the iron-based amorphous magnetic core includes at least one of Fe73.5Si15.5B7Cu1Nb3、Fe73.5Si13.5B9Cu1Nb3、Fe63.5Ni10Si15.5B7Cu1Nb3、Fe63.5Co5Ni5Si15.5B7Cu1Nb3、Fe68.5Co5Si15.5B7Cu1Nb3.
The method is a heat treatment method, has effects on various iron-based alloys, is suitable for different types of amorphous magnetic cores, and is particularly suitable for the iron-based amorphous magnetic cores with the element content range, so that the magnetic cores prepared from the iron-based amorphous magnetic cores have effective magnetic permeability lower than 1500 at 1-100 KHz.
Preferably, in the step (1), the heating rate of the iron-based amorphous magnetic core when heated to a preset temperature is 5-30 ℃ per minute.
The heating rate influences the time for heating the iron-based amorphous magnetic core to the preset temperature, the larger the heating rate is, the shorter the required heating time is, the preset temperature of heat treatment can be reached more quickly, the excessive growth of the size of crystal grains in the magnetic core in the heating process is avoided, and the magnetic conductivity and the stability of the magnetic core cannot be controlled effectively. At the above-mentioned heating rate, the core can be made to have an effective permeability of less than 1500 at 1-100 KHz.
Preferably, in the step (1), the cooling rate of the cooling is 50-1000 ℃ per minute.
After the preset temperature and pressure are reached, the magnetic core starts to be cooled, the natural cooling temperature rate along with the furnace is generally 6-8 ℃ per minute, and is higher than the cooling rate in the range, the cooling rate in the range is realized by equipment for assisting rapid quenching, the magnetic core can be rapidly cooled, the residence time of the magnetic core at a higher temperature is shortened, the excessive growth of crystal grains in the magnetic core is avoided, the size of recrystallized crystal grains is effectively controlled, and the finally prepared magnetic core keeps lower magnetic conductivity and higher stability.
Preferably, the pressurizing means includes at least one of pressurizing by an inert gas pressure and pressurizing by die extrusion. Further preferably, the inert gas includes at least one of argon and nitrogen.
Preferably, the temperature of the magnetic field heat treatment is 300-380 ℃, and the magnetic field strength of the magnetic field heat treatment is 800-3000Gs.
Preferably, the time of the magnetic field heat treatment is 1 to 120min, and more preferably 30 to 60min.
The higher the magnetic field strength, the higher the heat treatment temperature, the longer the heat preservation time, the greater the degree of induced grain-oriented growth, the lower the permeability, the higher the permeability stability, but the higher the magnetic field strength, the higher the heat treatment temperature, the longer the heat preservation time, not only significantly increases the actual production cycle, cost and equipment loss, but also the degree of induced grain-oriented growth by the heat treatment of the magnetic field can be reduced, and the long-term high-temperature growth can cause excessive growth of nano grains, resulting in the increase of permeability and the reduction of the permeability stability. Therefore, under the magnetic field heat treatment condition in the above range, the magnetic core of the present invention can achieve the purpose of maintaining lower magnetic permeability and higher stability.
Preferably, in the step (1), the iron-based amorphous magnetic core is wound from an iron-based amorphous ribbon.
Preferably, the magnetic field direction of the magnetic field heat treatment in step (2) is parallel to the width direction of the iron-based amorphous strip.
Preferably, in step (2), the cooling is natural cooling.
Preferably, the magnetic permeability of the iron-based magnetic core is constant at the frequency of 1-100kHz, the magnetic permeability of the iron-based magnetic core is 1500-14999, and the iron-based magnetic core contains amorphous phase and nano-sized crystal grains.
Further preferably, when the magnetic permeability of the iron-based magnetic core is constant, the change rate of the effective magnetic permeability of the iron-based magnetic core is equal to or less than 5% at a frequency of 1 to 100 kHz.
The invention also provides application of the iron-based magnetic core in preparation of an inductor and a high-current power device.
Compared with the prior art, the method has the beneficial effects that the iron-based amorphous magnetic core can be obtained through the heat treatment of the force field and the magnetic field of specific temperature and pressure and the heat treatment of the magnetic field, and the iron-based magnetic core has the characteristic of less than 1500 and constant magnetic conductivity at 1-100 kHz.
Drawings
Fig. 1 is an X-ray diffraction (XRD) pattern of a homemade amorphous ribbon.
FIG. 2 is a physical diagram of the magnetic core produced in example 1.
Fig. 3 is a diagram showing the comparison of magnetic domain structures between example 1 (left) and comparative example 3 (right).
Fig. 4 is a graph showing the relationship between effective permeability and frequency of the iron-based nanocrystalline magnetically soft alloy cores of examples 1 to 16.
Fig. 5 is a graph showing the relationship between effective permeability and frequency of the iron-based nanocrystalline magnetically soft alloy cores of comparative examples 1-7.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described by means of specific examples. The test methods used in examples and/or comparative examples are conventional methods unless otherwise specified, and materials, reagents and the like used, unless otherwise specified, are commercially available.
The amorphous strips adopted in the following examples and comparative examples are purchased in the market and can also be obtained by self-made by a conventional method, and the self-made method can comprise the following steps of (1) proportioning components, (2) smelting master alloy, and (3) carrying out strip casting and strip winding to obtain the corresponding amorphous strips.
Example 1
A method for preparing an iron-based magnetic core, comprising the steps of:
(1) Winding an amorphous alloy Fe 73.5Si15.5B7Cu1Nb3 strip (self-made, XRD result of which is shown as figure 1) by atom percentage into an amorphous magnetic core, placing the amorphous magnetic core in a furnace body, vacuumizing, filling inert gas argon so that certain pressure exists in the system, heating to the temperature of 350 ℃ for heat treatment of a force field at the heating rate of 15 ℃ per minute, continuously filling argon to the preset pressure of 130MPa, cooling at the cooling rate of 100 ℃ per minute, and then starting to release the pressure until the room temperature and normal pressure are reached to obtain a presintered magnetic core;
(2) And placing the presintered magnetic core in the magnetic field heat treatment furnace, heating to the magnetic field heat treatment temperature of 350 ℃ at the heating rate of 10 ℃ per minute, applying a magnetic field parallel to the width direction of the magnetic core, carrying out heat preservation for 60 minutes under the action of the magnetic field strength of 1000Gs, and cooling to the room temperature along with the furnace to obtain the iron-based magnetic core.
Examples 2 to 15 and comparative examples 1 to 7
Examples 2 to 15 and comparative examples 1 to 7 differ from example 1 only in the rate of rise and fall of temperature, the heat treatment temperature of the force field, the preset pressure, the strength of the magnetic field, the heat treatment temperature of the magnetic field or the holding time in steps (1) to (2), and the detailed differences are shown in Table 1.
Example 16
The difference between the present embodiment 1 and the embodiment is that the alloy of the present embodiment is an amorphous ribbon of Fe 73.5Si13.5B9Cu1Nb3 in atomic percent, and the amorphous ribbon is the same as the amorphous ribbon of embodiment 1 obtained by a commercially available method or a self-made method by a conventional method, and the self-made method of the present embodiment and embodiment 1 may include the steps of (1) component proportioning, (2) master alloy melting, and (3) ribbon winding by a ribbon-casting and ribbon winding to obtain the corresponding amorphous ribbon.
TABLE 1
The iron-based magnetic cores prepared in the examples and the comparative examples were subjected to performance test, wherein the inductance L of the magnetic core was measured by using a KEYSIGHT AGILENT 4294A precision impedance analyzer at an applied magnetic field of 1A/m and a frequency range of 1kHz to 100kHz, and the effective permeability μ e was obtained by an inductance L conversion formula:
μe=(L×Le)/(N2×Ae),
Wherein L is the magnetic core inductance, mu e is the magnetic core effective magnetic permeability, L e is the magnetic path length of the magnetic core, A e is the magnetic core effective sectional area, and N is the number of turns of the coil (the test condition is 1 turn).
Mu e% change rate was calculated by mu e% change rate= (mu e(1kHz)e(100kHz))/μe(1kHz) ×100), and mu e% change rate less than 5% in the present invention was regarded as constant permeability.
TABLE 2
As can be seen from examples 1-16 and comparative examples 1-7 by combining the heat treatments of the force field and the magnetic field and requiring heat treatment at a specific temperature and pressure, the present invention can provide an iron-based core having a low, stable or constant effective permeability in the range of 100-1499 at 1-100KHz, as can be seen from the analysis of table 2 and fig. 2, 4-5.
In the method, under the heat treatment of the force field, the speed of rising/reducing temperature, the heat treatment temperature, the heat preservation time and the pressure can all have certain influence on the magnetic permeability and the stability of the magnetic permeability of the iron-based nanocrystalline magnetic core. This is because, on the one hand, pressure forces the nanocrystalline grains to precipitate but at the same time inhibits the nanocrystalline grains from growing rapidly, to a certain extent, by controlling the grain size, the core is kept at a relatively low permeability and a relatively stable permeability, and, on the other hand, the presence of the pressure field can induce magnetic anisotropy inside the core, increasing domain wall energy, while a high domain wall can inhibit domain wall movement, to a certain extent, by controlling the domain wall, the core permeability is relatively low and the permeability is relatively stable. The object of the invention is to achieve a constant effective permeability of 100-1499 at 1-100KHz for the purpose of application in a specific field. It can be seen from the above examples 1-3, 8-9, and 16 that the magnetic properties required by the present invention can be achieved in a relatively wide range under a thermal field, with a heating rate of 5-30 ℃ per minute, a cooling rate of 50-1000 ℃ per minute, and different kinds of amorphous cores. The temperature rising rate and the temperature reducing rate belong to the degree of rapid heating and rapid cooling in the field of industrial production, the time of a magnetic core in the heat treatment process is shortened, the phenomenon that the magnetic permeability and the stability of the magnetic core are unqualified due to excessive growth of crystal grains in the magnetic core is avoided, and particularly in the cooling process, the natural cooling temperature rate along with a furnace is generally 6-8 ℃ per minute and is higher than the cooling rate in the range, and the auxiliary rapid quenching equipment is needed. From examples 1, 4-7 and comparative examples 1, 4-7, the effect of the temperature and pressure of the heat treatment of the force field on the permeability and its stability is very pronounced. Under the heat treatment of a force field at 300-425 ℃, the magnetic core can still keep relatively low magnetic permeability and relatively stable magnetic permeability, but slightly deviate from the temperature range, the magnetic permeability is overlarge and the magnetic permeability stability is drastically reduced due to the high temperature, and the magnetic permeability stability is drastically reduced although the magnetic permeability meets the requirement, but the magnetic permeability stability is not met. The magnetic core can maintain relatively low magnetic permeability and relatively stable magnetic permeability under the pressure of a force field with the pressure of 60-150MPa, but the magnetic permeability of the magnetic core is slightly deviated from the pressure range, and the magnetic permeability of the magnetic core meets the requirement, but the stability of the magnetic permeability cannot meet the requirement. Therefore, the thermal field of the invention is actually a heat treatment mode of rapid heating and rapid cooling, under the synergistic effect of specific temperature and high pressure, the nano crystal grains are promoted to be continuously precipitated, the growth of the nano crystal grains is restrained, the crystal grain state and size in the magnetic core are controlled, the domain wall energy is improved to a certain extent, and the performance effects of low magnetic conductivity and constant magnetic conductivity of the magnetic core are integrally realized.
Under the heat treatment of a magnetic field, the magnetic field strength, the heat preservation time and the heat treatment temperature can have certain influence on the magnetic permeability and the stability of the iron-based nanocrystalline magnetic core. This is because the magnetic field heat treatment actually acts to induce grain-oriented growth, that is, to induce orientation of the nano-grains in the direction of magnetic field application, thereby inducing magnetic anisotropy and regulating the hysteresis loop shape. From the above examples 1, 10-15, it is known that the magnetic field heat treatment temperature is 300-380 ℃, the magnetic field strength is 800-3000Gs, the holding time is 30-120min, the higher the magnetic field strength, the higher the heat treatment temperature, the longer the holding time, the greater the extent of induced grain-oriented growth, the lower the permeability, the higher the permeability stability, but the higher the magnetic field strength, the higher the heat treatment temperature, the longer the holding time not only significantly increases the actual production cycle, cost and equipment loss, but also the extent of induced grain-oriented growth by the magnetic field heat treatment decreases, and the long-term high-temperature growth causes excessive growth of nano-crystal grains, resulting in increased permeability and decreased stability of permeability, therefore, the conditions of the magnetic field heat treatment of the present invention are preferably in the parameter ranges of 300-380 ℃, the magnetic field strength is 800-3000Gs, and the holding time is 30-120min.
As is clear from examples 1 and comparative examples 1 to 3, the force field heat treatment and the magnetic field heat treatment are mutually matched, and the grain orientation growth is induced by the magnetic field heat treatment under the basis of adjusting and controlling the grain and domain wall energy by the force field heat treatment, so that the prepared magnetic core cannot maintain the performance of low frequency and low constant magnetic permeability under any condition of lacking the condition of pressurizing more than atmospheric pressure or the condition of adding a constant magnetic field.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.

Claims (10)

1. A method for preparing an iron-based magnetic core, comprising the steps of:
(1) Heating the iron-based amorphous magnetic core to a preset temperature and simultaneously pressurizing to a preset pressure, and then cooling to below 200 ℃ to start releasing the pressure to obtain a presintered magnetic core, wherein the preset temperature is 300-425 ℃, and the preset pressure is 60-150MPa;
(2) And performing magnetic field heat treatment on the presintered magnetic core, and cooling to obtain the iron-based magnetic core.
2. The method of manufacturing an iron-based magnetic core according to claim 1, wherein in the step (1), a heating rate when the iron-based amorphous magnetic core is heated to a predetermined temperature is 5 to 30 ℃.
3. The method of claim 1, wherein in the step (1), the cooling rate is 50-1000 ℃ per minute, and the pressurizing means comprises at least one of pressurizing by gas pressure and pressurizing by die extrusion.
4. The method of manufacturing an iron-based magnetic core according to claim 1, wherein in the step (2), the temperature of the magnetic field heat treatment is 300 to 380 ℃, and the magnetic field strength of the magnetic field heat treatment is 800 to 3000Gs.
5. The method of manufacturing an iron-based magnetic core according to claim 1, wherein in the step (2), the time of the magnetic field heat treatment is 1 to 120 minutes, and the cooling is natural cooling.
6. The method of manufacturing an iron-based magnetic core according to claim 1, wherein the iron-based amorphous magnetic core in step (1) is wound from an iron-based amorphous strip, and the magnetic field direction of the magnetic field heat treatment in step (2) is parallel to the width direction of the iron-based amorphous strip.
7. The method of manufacturing an iron-based magnetic core according to claim 1, wherein in the step (1), the iron-based amorphous magnetic core includes, in atomic percentage, 60-80% of Fe, 10-20% of Si, 0-10% of B, 0-3% of Cu, 0-5% of Nb, 0-15% of Ni, and 0-10% of Co.
8. An iron-based magnetic core produced by the method for producing an iron-based magnetic core according to any one of claims 1 to 7.
9. The iron-based magnetic core according to claim 8, wherein the iron-based magnetic core has a constant magnetic permeability at a frequency of 1 to 100kHz and a magnetic permeability of 100 to 1499, and the iron-based magnetic core contains amorphous phase and nano-sized crystal grains.
10. Use of the iron-based core according to claim 8 or 9 for the manufacture of an inductor, a high current power device.
CN202411588568.XA 2024-11-08 2024-11-08 A kind of iron-based magnetic core with constant low magnetic permeability and its preparation method Pending CN119252643A (en)

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