CN118866492B - Composite magnetic material and its preparation method and application - Google Patents
Composite magnetic material and its preparation method and application Download PDFInfo
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- H—ELECTRICITY
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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Abstract
The invention relates to a composite magnetic material and a preparation method and application thereof, wherein the composite magnetic material comprises a magnetic framework, the magnetic field intensity of the magnetic framework is gradually increased from the center to the edge, the magnetic field intensity of the edge is different from the magnetic field intensity of the center by more than 100 gauss, composite magnetic powder filled in the magnetic framework is at least divided into three layers in the direction from the center to the edge of the magnetic framework, the difference value of the magnetic permeability of the composite magnetic powder of the innermost layer and the magnetic permeability of the composite magnetic powder of the outermost layer is more than 500, the magnetic permeability of the composite magnetic powder is gradually increased or gradually decreased according to the layers, and the particle size of the composite magnetic powder is gradually increased according to the layers. The composite magnetic material has high magnetic permeability in the frequency range of 1kHz-1GHz, and electromagnetic performance parameters are wide and dynamically adjustable, so that the composite magnetic material can be compatible in high-frequency environment and low-frequency environment.
Description
Technical Field
The invention relates to the technical field of electromagnetic wave-absorbing materials, in particular to a composite magnetic material and a preparation method and application thereof.
Background
With the rise of new energy fields such as photovoltaics, charging piles, automobile electronics and the like, high-power equipment with high voltage, high frequency and large through current is widely applied, and the strong magnetic field or electromagnetic radiation generated by the high-power equipment can seriously interfere the normal operation of surrounding electronic equipment, so that the performance of the electronic equipment is reduced, the data transmission is abnormal and even the equipment is failed. At present, the absorption and shielding of corresponding electromagnetic waves are generally performed by a device made of a magnetic material, however, the conventional magnetic material has high magnetic permeability only in a specific frequency band, so that the application field of the conventional magnetic material is limited, and the compatible use of a high-frequency environment and a low-frequency environment cannot be realized.
Disclosure of Invention
Based on the above, it is necessary to provide a composite magnetic material, a preparation method and application thereof, wherein the composite magnetic material has high magnetic permeability in the frequency range of 1kHz-1GHz, and electromagnetic performance parameters are wide and dynamically adjustable, so that compatible use in high-frequency environment and low-frequency environment is realized.
The invention discloses a composite magnetic material, which comprises the following components:
The magnetic skeleton is characterized by comprising a magnetic field intensity which is gradually increased from the center to the edge, wherein the magnetic field intensity of the edge is different from that of the center by more than 100 gauss;
The composite magnetic powder filled in the magnetic framework is divided into at least three layers in the direction from the center to the edge of the magnetic framework, wherein the difference value of the magnetic permeability of the innermost composite magnetic powder and the magnetic permeability of the outermost composite magnetic powder is larger than 500, the magnetic permeability of the composite magnetic powder is gradually increased or gradually decreased according to the layers, and the particle size of the composite magnetic powder is gradually increased according to the layers.
In one embodiment, when the magnetic permeability of the composite magnetic powder is gradually increased according to the level, the magnetic permeability of the composite magnetic powder of the innermost layer is 500-1500, and the magnetic permeability of the composite magnetic powder of the outermost layer is 2500-3500;
When the magnetic permeability of the composite magnetic powder is gradually reduced according to the level, the magnetic permeability of the composite magnetic powder of the innermost layer is 2500-3500, and the magnetic permeability of the composite magnetic powder of the outermost layer is 500-1500.
In one embodiment, the particle size of the composite magnetic powder of the innermost layer is 500nm to 700nm, and the particle size of the composite magnetic powder of the outermost layer is 1200nm to 1500nm.
In an embodiment, the composite magnetic powder is selected from at least three of zinc-based composite magnetic powder, iron-based composite magnetic powder, magnesium-based composite magnetic powder, manganese-based composite magnetic powder, or nickel-based composite magnetic powder.
In one embodiment, the composite magnetic powder satisfies at least one of the following conditions:
(1) The magnetic permeability of the zinc-based composite magnetic powder is 500-1500, and the particle size is 500-700 nm or 1200-1500 nm;
(2) The magnetic permeability of the iron-based composite magnetic powder is 1200-2100, and the particle size is 600nm-900nm or 1000nm-1300nm;
(3) The magnetic permeability of the magnesium-based composite magnetic powder is 1500-2400, and the particle size is 800-1100 nm;
(4) The magnetic permeability of the manganese-based composite magnetic powder is 2100-2800, and the particle size is 1000nm-1300nm or 600nm-900nm;
(5) The magnetic permeability of the nickel-based composite magnetic powder is 2500-3500, and the particle size is 1200nm-1500nm or 500nm-700nm.
In an embodiment, in a direction from the center to the edge of the magnetic framework, the magnetic framework is sequentially filled with zinc-based composite magnetic powder, iron-based composite magnetic powder, magnesium-based composite magnetic powder, manganese-based composite magnetic powder and nickel-based composite magnetic powder;
Or the magnetic skeleton is sequentially filled with iron-based composite magnetic powder, magnesium-based composite magnetic powder and nickel-based composite magnetic powder;
or in the direction from the center to the edge of the magnetic framework, zinc-based composite magnetic powder, manganese-based composite magnetic powder and nickel-based composite magnetic powder are sequentially filled in the magnetic framework;
or in the direction from the center to the edge of the magnetic framework, zinc-based composite magnetic powder, magnesium-based composite magnetic powder and nickel-based composite magnetic powder are sequentially filled in the magnetic framework;
Or the nickel-based composite magnetic powder, the manganese-based composite magnetic powder, the magnesium-based composite magnetic powder, the iron-based composite magnetic powder and the zinc-based composite magnetic powder are sequentially filled in the magnetic framework from the center to the edge of the magnetic framework;
Or in the direction from the center to the edge of the magnetic framework, the manganese-based composite magnetic powder, the magnesium-based composite magnetic powder and the iron-based composite magnetic powder are sequentially filled in the magnetic framework.
In one embodiment, the magnetic field strength at the center of the magnetic skeleton is greater than or equal to 30 gauss, and the magnetic field strength at the edges of the magnetic skeleton is less than or equal to 200 gauss;
And/or the aperture of the magnetic framework is 4-5 times of the maximum particle size of the composite magnetic powder.
In one embodiment, the magnetic framework is selected from magnetic iron oxide frameworks.
In an embodiment, the mass ratio of the magnetic framework to the composite magnetic powder is 2:1-5:1, and the mass ratio between the composite magnetic powder of any two layers is 1:2-2:1.
In the composite magnetic material provided by the invention, the composite magnetic powder is filled in the magnetic framework according to the specific level sequence of particle size and magnetic permeability, so that the composite magnetic material has high magnetic permeability in the frequency band of 1kHz-1GHz, and the current flowing direction can be carried out according to the lowest impedance loop. Therefore, when the composite magnetic material is applied to the electronic equipment for electromagnetic wave absorption and shielding, the composite magnetic material can well reduce energy loss and electromagnetic interference in a high-frequency environment and a low-frequency environment, so that the composite magnetic material can be used in a high-frequency environment and a low-frequency environment in a compatible manner, the electronic equipment can be further used in the high-frequency environment and the low-frequency environment in a compatible manner, the electronic equipment is protected from external electromagnetic interference, and in addition, the type and the arrangement sequence of the composite magnetic material can be changed, the key magnetic focusing frequency range of the composite magnetic material can be regulated, and the wide dynamic regulation of the electromagnetic performance of the composite magnetic material can be realized, so that the composite magnetic material is applied to specific scenes.
The preparation method of the composite magnetic material comprises the following steps:
providing at least three kinds of composite magnetic powder, wherein the particle sizes and the grades of magnetic permeability of the composite magnetic powder are different;
Providing a magnetic framework, wherein the aperture of the magnetic framework is larger than the maximum particle size of the composite magnetic powder;
and mixing the magnetic framework with the composite magnetic powder in sequence according to the particle size grade and the magnetic permeability grade of the composite magnetic powder, so that the composite magnetic powder is filled in the magnetic framework in sequence, and a composite magnetic material is obtained.
In one embodiment, the method for preparing the composite magnetic powder includes:
Under the protection of inert gas, mixing a metal simple substance with a metal oxide, performing heating reaction, then further mixing with silicon, and cooling to obtain a solidification product, wherein the metal simple substance is selected from one of iron, zinc, nickel, manganese or magnesium, and the metal oxide comprises at least one of ferric oxide, manganese oxide, zinc oxide, nickel oxide or magnesium oxide;
Crushing the solidified product to obtain a crushed product, and classifying the crushed product according to particle size grades to obtain magnetic powder raw materials with different particle size grades;
And (3) placing the magnetic powder raw materials in an electromagnetic environment for magnetization to obtain the composite magnetic powder.
In one embodiment, the magnetic powder raw material is placed in an electromagnetic environment for magnetization,
When the metal simple substance is selected from zinc, the magnetic field strength is 90 gauss-110 gauss;
when the metal simple substance is selected from iron, the magnetic field strength is 140 gauss-150 gauss;
when the metal simple substance is selected from magnesium, the magnetic field strength is 50 gauss-65 gauss;
when the metal simple substance is selected from manganese, the magnetic field strength is 70 gauss-80 gauss;
when the metal simple substance is selected from nickel, the magnetic field strength is 120 gauss-130 gauss.
In one embodiment, the method for preparing the magnetic skeleton comprises:
Pressurizing and heating the ferric oxide under the protection of inert gas to obtain a heated product, wherein in the pressurizing step, the pressure is linearly increased;
Applying a mist coagulant to the heated product to obtain a skeleton;
And magnetizing the framework to obtain the magnetic framework.
In one embodiment, in the step of magnetizing the former, the magnetic field strength increases in a direction from the center to the edge of the former.
According to the preparation method of the composite magnetic material, the magnetic framework is sequentially mixed with the composite magnetic powder according to the particle size level and the magnetic permeability level of the composite magnetic powder, so that the composite magnetic powder is sequentially filled in the magnetic framework, and the simple preparation of the composite magnetic material with high magnetic permeability in the frequency range of 1kHz-1GHz is realized.
An application of the composite magnetic material in electronic equipment.
The composite magnetic material has high magnetic permeability in the frequency range of 1kHz-1GHz, and electromagnetic performance parameters are wide and dynamically adjustable, so that the electronic equipment can be protected from external electromagnetic interference when the composite magnetic material is applied to the electronic equipment, the compatible use of the electronic equipment in a high-frequency environment and a low-frequency environment is realized, and in addition, the adaptive composite magnetic material can be selected according to the characteristics of different electronic equipment and is applied to a specific scene.
Drawings
FIG. 1 is a high-power scanning electron microscope image of the iron-based composite magnetic powder prepared in example 1;
FIG. 2 is a high power scanning electron microscope image of the composite magnetic material prepared in example 1;
Fig. 3 is a graph showing the relationship between the magnetic permeability and the frequency of the composite magnetic material prepared in example 1.
Detailed Description
The present invention will be described in more detail below in order to facilitate understanding of the present invention. It should be understood, however, that the invention may be embodied in many different forms and should not be limited to the implementations or embodiments described herein. Rather, these embodiments or examples are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments or examples only and is not intended to be limiting of the invention. As used herein, the optional scope of the term "and/or" includes any one of the two or more related listed items, as well as any and all combinations of related listed items, including any two or more of the related listed items, or all combinations of related listed items.
The present invention provides a composite magnetic material comprising:
the magnetic field intensity of the magnetic framework gradually increases from the center to the edge, and the magnetic field intensity of the edge is different from the magnetic field intensity of the center by more than 100 gauss;
The composite magnetic powder filled in the magnetic framework is at least divided into three layers in the direction from the center to the edge of the magnetic framework, wherein the difference value of the magnetic permeability of the composite magnetic powder of the innermost layer and the magnetic permeability of the composite magnetic powder of the outermost layer is larger than 500, the magnetic permeability of the composite magnetic powder is gradually increased or gradually decreased according to the layers, and the particle size of the composite magnetic powder is gradually increased according to the layers.
It should be noted that, when the magnetic permeability of the composite magnetic powder in the same level is within 200, the particle size of the composite magnetic powder in the same level is within 150nm, and the gradual increase or decrease may be a regular gradient increase or decrease or an irregular increase or decrease, preferably, the magnetic permeability of the composite magnetic powder is increased or decreased according to the level gradient, and the particle size of the composite magnetic powder is increased according to the level gradient.
In the composite magnetic material provided by the invention, the composite magnetic powder is filled in the magnetic framework according to the specific level sequence of particle size and magnetic permeability, so that the composite magnetic material has high magnetic permeability in the frequency band of 1kHz-1GHz, and the current flowing direction can be carried out according to the lowest impedance loop.
Therefore, when the composite magnetic material is applied to the electronic equipment for electromagnetic wave absorption and shielding, the composite magnetic material can well reduce energy loss and electromagnetic interference in a high-frequency environment and a low-frequency environment, so that the compatible use of the composite magnetic material in the high-frequency environment and the low-frequency environment is realized, the compatible use of the electronic equipment in the high-frequency environment and the low-frequency environment is further realized, and the electronic equipment is protected from the influence of external electromagnetic interference;
In addition, the type and the arrangement sequence of the composite magnetic material can be changed, so that the key magnetic focusing frequency band of the composite magnetic material can be adjusted, and the wide dynamic adjustment of the electromagnetic performance of the composite magnetic material can be realized, thereby being applied to specific scenes.
In an embodiment, the composite magnetic powder is selected from an iron-based composite magnetic powder, a zinc-based composite magnetic powder, a nickel-based composite magnetic powder, a manganese-based composite magnetic powder or a magnesium-based composite magnetic powder.
Because the composite magnetic powder has specific chemical components and microstructures, the magnetic permeability of different types of composite magnetic powder is fixed relative to the size, and in one embodiment, the arrangement sequence of the composite magnetic powder is zinc-based composite magnetic powder, iron-based composite magnetic powder, magnesium-based composite magnetic powder, manganese-based composite magnetic powder and nickel-based composite magnetic powder according to the magnetic permeability from small to large; preferably, the magnetic permeability of the zinc-based composite magnetic powder is 500 to 1500, including but not limited to 500, 600, 700, 800, 900, 1000, 1100, 1200, 1300, 1400 or 1500, the magnetic permeability of the iron-based composite magnetic powder is 1200 to 2100, including but not limited to 1200, 1300, 1400, 1500, 1600, 1700, 1800, 1900, 2000 or 2100, the magnetic permeability of the magnesium-based composite magnetic powder is 1500 to 2400, including but not limited to 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300 or 2400, the magnetic permeability of the manganese-based composite magnetic powder is 2100 to 2800, including but not limited to 2100, 2200, 2300, 2400, 2500, 2600, 2700 or 2800, 2500 to 3500, including but not limited to 2500, 2600, 2700, 3000, 3100, 3200, 3300, 3400 or 3500.
When the magnetic permeability of the composite magnetic powder is gradually increased according to the level, the composite magnetic material has high insertion loss characteristics, so that when the composite magnetic material is applied to electronic equipment, the function of filtering the electronic equipment can be improved, the composite magnetic material is suitable for a power input port filtering application scene, preferably, the magnetic permeability of the innermost composite magnetic powder is 500-1500, including but not limited to 500, 600, 700, 800, 900, 1000, 1100, 1200, 1300, 1400 or 1500, the magnetic permeability of the outermost composite magnetic powder is 2500-3500, including but not limited to 2500, 2600, 2700, 2800, 2900, 3000, 3100, 3200, 3300, 3400 or 3500, and further preferably, the magnetic permeability of the innermost composite magnetic powder is 900-1100, and the magnetic permeability of the outermost composite magnetic powder is 3200-3400.
When the magnetic permeability of the composite magnetic powder is gradually reduced according to the level, the composite magnetic material has high-pass magnetic characteristics, so that when the composite magnetic material is applied to electronic equipment, the electromagnetic transmission efficiency can be improved, the composite magnetic material is suitable for power supply voltage transformation application scenes, preferably, the magnetic permeability of the innermost composite magnetic powder is 2500-3500 including but not limited to 2500, 2600, 2700, 2800, 2900, 3000, 3100, 3200, 3300, 3400 or 3500, the magnetic permeability of the outermost composite magnetic powder is 500-1500 including but not limited to 500, 600, 700, 800, 900, 1000, 1100, 1200, 1300, 1400 or 1500, further preferably, the magnetic permeability of the innermost composite magnetic powder is 3200-3400, and the magnetic permeability of the outermost composite magnetic powder is 900-1000.
In order to better pack various composite magnetic materials within the magnetic skeleton, in one embodiment, the particle size of the composite magnetic powder closest to the center of the magnetic skeleton is 500nm to 700nm, and the particle size of the composite magnetic powder furthest from the center of the magnetic skeleton is 1200nm to 1500nm. It is understood that the particle size of the composite magnetic powder is related to the position thereof in the composite magnetic material, when the magnetic permeability of the composite magnetic powder is gradually increased in the order of the layers, the particle size of the zinc-based composite magnetic powder is 500nm to 700nm, the particle size of the iron-based composite magnetic powder is 600nm to 900nm, the particle size of the magnesium-based composite magnetic powder is 800nm to 1100nm, the particle size of the manganese-based composite magnetic powder is 1000nm to 1300nm, the particle size of the nickel-based composite magnetic powder is 1200nm to 1500nm, and when the magnetic permeability of the composite magnetic powder is gradually decreased in the order of the layers, the particle size of the nickel-based composite magnetic powder is 500nm to 700nm, the particle size of the manganese-based composite magnetic powder is 600nm to 900nm, the particle size of the magnesium-based composite magnetic powder is 800nm to 1000nm, the particle size of the iron-based composite magnetic powder is 1000nm to 1300nm, and the particle size of the zinc-based composite magnetic powder is 1200nm to 1500nm.
In one embodiment, the mass ratio of the magnetic skeleton to the composite magnetic powder is 2:1-5:1, including but not limited to 2:1, 3:1, 4:1, or 5:1, and the mass ratio between any two levels of composite magnetic powder is 1:2-2:1, including but not limited to 1:2, 1:1.5, 1.5:1.5, 1.5:2, 2:1.5, 1.5:1, 2:1.
In one embodiment, the magnetic framework is selected from magnetic iron oxide frameworks.
In order to more completely fill the composite magnetic powder into the magnetic skeleton, in one embodiment, the pore size of the magnetic skeleton is 4-5 times the maximum particle size of the composite magnetic powder, including but not limited to 4.1 times, 4.2 times, 4.3 times, 4.4 times, 4.5 times, 4.6 times, 4.7 times, 4.8 times, 4.9 times, or 5.0 times.
In order to make the composite magnetic powder more stably filled in the magnetic skeleton, in an embodiment, the magnetic field intensity of the center of the magnetic skeleton is greater than or equal to 30 gauss, including but not limited to 30 gauss, 40 gauss, 50 gauss, 60 gauss, 70 gauss, 80 gauss, 90 gauss or 100 gauss, and the magnetic field intensity of the edge of the magnetic skeleton is less than or equal to 200 gauss, including but not limited to 200 gauss, 190 gauss, 180 gauss, 170 gauss, 160 gauss, 150 gauss, 140 gauss or 130 gauss.
In a specific embodiment, the zinc-based composite magnetic powder, the iron-based composite magnetic powder, the magnesium-based composite magnetic powder, the manganese-based composite magnetic powder and the nickel-based composite magnetic powder are sequentially filled in the magnetic framework from the center to the edge of the magnetic framework, at this time, the magnetic permeability of the composite magnetic material in the frequency band of 1kHz-1GHz reaches more than 2100, the insertion loss reaches more than 3dB, and when the composite magnetic material is applied to electronic equipment, the electromagnetic compatibility disturbance suppression function can be improved, and the composite magnetic material is suitable for application scenes of power supply filtering.
In a specific embodiment, the iron-based composite magnetic powder, the magnesium-based composite magnetic powder and the nickel-based composite magnetic powder are sequentially filled in the magnetic framework from the center to the edge of the magnetic framework, at this time, the magnetic permeability of the composite magnetic material in a frequency band of 1kHz-1GHz reaches more than 2100, the important magnetic focusing frequency band is 150kHz-200MHz, the insertion loss reaches more than 4dB, and when the composite magnetic material is applied to electronic equipment, the electromagnetic compatibility disturbance suppression function can be improved, and the composite magnetic material is suitable for application scenes of power supply filtering.
In a specific embodiment, zinc-based composite magnetic powder, manganese-based composite magnetic powder and nickel-based composite magnetic powder are sequentially filled in the magnetic framework from the center to the edge of the magnetic framework, at this time, the magnetic permeability of the composite magnetic material in the frequency band of 1kHz-1GHz reaches above 1900, the key magnetic focusing frequency band of the composite magnetic material is 30MHz-1GHz, the insertion loss reaches above 3dB, and when the composite magnetic material is applied to electronic equipment, the function of radiation disturbance suppression can be improved, and the composite magnetic material is suitable for equipment radiation disturbance exceeding application scenes.
In a specific embodiment, nickel-based composite magnetic powder, manganese-based composite magnetic powder, magnesium-based composite magnetic powder, iron-based composite magnetic powder and zinc-based composite magnetic powder are sequentially filled in the magnetic framework from the center to the edge of the magnetic framework, at this time, the magnetic permeability of the composite magnetic material in the frequency range of 1kHz-1GHz reaches above 2400, the focused magnetic frequency range of the composite magnetic material is 30kHz-900MHz, and when the composite magnetic material is applied to electronic equipment, the function of improving the power supply filtering efficiency can be improved, and the composite magnetic material is suitable for application scenes of power supply module filtering.
In a specific embodiment, nickel-based composite magnetic powder, manganese-based composite magnetic powder and iron-based composite magnetic powder are sequentially filled in the magnetic framework from the center to the edge of the magnetic framework, at this time, the magnetic permeability of the composite magnetic material in the frequency band of 1kHz-1GHz reaches more than 1800, the key magnetic focusing frequency band of the composite magnetic material is 100kHz-2MHz, and the magnetic flux efficiency is as high as 97% or more.
In a specific embodiment, the manganese-based composite magnetic powder, the magnesium-based composite magnetic powder and the iron-based composite magnetic powder are sequentially filled in the magnetic framework from the center to the edge of the magnetic framework, at this time, the magnetic permeability of the composite magnetic material in the frequency range of 1kHz-1GHz reaches more than 1500, the key magnetic focusing frequency range of the composite magnetic material is 500kHz-5MHz, and the magnetic flux efficiency is as high as 95% or more.
The invention also provides a preparation method of the composite magnetic material, which comprises the following steps:
s10, providing at least three kinds of composite magnetic powder, wherein the particle sizes and the grades of the magnetic permeability of the composite magnetic powder are different;
S20, providing a magnetic framework, wherein the aperture of the magnetic framework is larger than the maximum particle size of the composite magnetic powder;
S30, mixing the magnetic framework with the composite magnetic powder in sequence according to the particle size grade and the magnetic permeability grade of the composite magnetic powder, so that the composite magnetic powder is filled in the magnetic framework in sequence, and the composite magnetic material is obtained.
According to the preparation method of the composite magnetic material, the magnetic framework is sequentially mixed with the composite magnetic powder according to the particle size grade and the magnetic permeability grade of the composite magnetic powder, so that the composite magnetic powder is sequentially filled in the magnetic framework, and the composite magnetic material with high magnetic permeability in the frequency range of 1kHz-1GHz is simply prepared.
In step S10, the composite magnetic powder is prepared from metal simple substance and metal oxide as raw materials mainly through high temperature, crushing and magnetization, and in one embodiment, the preparation method of the composite magnetic powder comprises the following steps:
S101, under the protection of inert gas, mixing a metal simple substance with a metal oxide, performing heating reaction, then further mixing with silicon, and cooling to obtain a solidification product;
s102, crushing a solidified product to obtain a crushed product, and classifying the crushed product according to particle size grades to obtain magnetic powder raw materials with different particle size grades;
s103, placing the magnetic powder raw materials in an electromagnetic environment for magnetization to obtain the composite magnetic powder.
In step S101, the metal simple substance is selected from one of iron, zinc, nickel, manganese or magnesium, and the metal oxide includes at least one of iron oxide, manganese oxide, zinc oxide, nickel oxide or magnesium oxide.
In one embodiment, the ratio of the mass of the elemental metal to the total mass of the metal oxides is from 5:4.5 to 3:5.
In one embodiment, the metal oxide comprises iron oxide, manganese oxide, zinc oxide, nickel oxide, and magnesium oxide, wherein the mass ratio of iron oxide, manganese oxide, zinc oxide, nickel oxide, and magnesium oxide is 0.5:1:1:1:1 to 1:1:1.
In the step of mixing the metal simple substance with the metal oxide and performing the heating reaction, the temperature is preferably 900-1500 ℃ and the time is preferably 1-3 h.
The addition of silicon can better realize the solidification of the heating product, so that the mass ratio of the metal simple substance to the silicon is preferably 10:1-15:1.
In the step S102, the pulverizing is performed at a rotation speed of preferably 300r/min to 500r/min and a pressure of preferably 150kPa to 250kPa.
In order to make the performance of the obtained composite magnetic material more stable, the crushed product needs to be subjected to impurity removal treatment after the crushing step, and the specific steps include washing the crushed product with a hydrogen peroxide solution.
In one embodiment, the crushed products are classified according to the particle size level by adopting a leaching method, and the specific steps comprise the steps of placing the crushed products in an aqueous solution for standing and layering, taking the crushed products positioned on the same layer to obtain the crushed products with the same particle size level, wherein the time of standing and layering is preferably 1.5-2.5 hours, and shaking and vibrating are carried out every 15-25 minutes in the standing and layering process to accelerate layering.
In step S103, in one embodiment, in the step of magnetizing the magnetic powder raw material in an electromagnetic environment, when the metal element is selected from zinc, the magnetic field strength is 90 to 110 gauss, preferably 98 to 102 gauss, when the metal element is selected from iron, the magnetic field strength is 140 to 150 gauss, preferably 143 to 147 gauss, when the metal element is selected from magnesium, the magnetic field strength is 50 to 65 gauss, preferably 58 to 62 gauss, when the metal element is selected from manganese, the magnetic field strength is 70 to 80 gauss, preferably 73 to 77 gauss, and when the metal element is selected from nickel, the magnetic field strength is 120 to 130 gauss, preferably 123 to 127 gauss.
In step S20, the magnetic skeleton is obtained by using iron oxide as a raw material and mainly through heating expansion and magnetization, and in one embodiment, the step of providing the magnetic skeleton includes:
S201, pressurizing and heating ferric oxide under the protection of inert gas to obtain a heated product, wherein in the pressurizing step, the pressure is linearly increased;
S202, applying a mist coagulant to the heated product to obtain a skeleton;
S203, magnetizing the framework to obtain the magnetic framework.
In step S201, the pressurizing is capable of avoiding crushing of the iron oxide during heating, and preferably, the pressurizing is increased from 3kPa to 7kPa to 40kPa to 70kPa, including but not limited to, from 3kPa to 40kPa, from 4kPa to 45kPa, from 5kPa to 50kPa, from 6kPa to 60kPa, and from 7kPa to 70kPa, and the rate of increase is 0.8kPa/5min to 1.2kPa/5min, including but not limited to 0.8kPa/5min, 0.9kPa/5min, 1.0kPa/5min, 1.1kPa/5min, or 1.2kPa/5min.
The temperature during the heating step is 200 ℃ to 300 ℃, including but not limited to 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃, 250 ℃, 260 ℃, 270 ℃, 280 ℃, 290 ℃, or 300 ℃.
In step S202, the step of applying a mist agent to the heated product includes atomizing the gel compound and spraying the gel compound onto the surface of the heated product.
In one embodiment, the mist coagulant comprises at least one of a silica gel, an alumina gel, or an iron hydroxide gel. In order to ensure uniform spray of the mist agent onto the framework without filling the framework, it is preferred that the mass ratio of heated product to mist agent is 15:1-10:1, including but not limited to 15:1, 14:1, 13:1, 12:1, 11:1 or 10:1.
In step S203, in the step of magnetizing the skeleton, the magnetic field strength increases from the center of the skeleton to the edge, specifically, the magnetic field strength of the skeleton center is 30 gauss to 50 gauss, including but not limited to 30 gauss, 32 gauss, 34 gauss, 36 gauss, 38 gauss, 40 gauss, 42 gauss, 44 gauss, 46 gauss, 48 gauss or 50 gauss, and the magnetic field strength of the edge is 170 gauss to 200 gauss, including but not limited to 170 gauss, 175 gauss, 180 gauss, 185 gauss, 190 gauss, 195 gauss or 200 gauss.
The invention also provides the application of the composite magnetic material in electronic equipment, such as common-mode inductance, transformer or differential-mode inductance, and the like, because the composite magnetic material has high magnetic permeability in the frequency range of 1kHz-1GHz, and electromagnetic performance parameters are wide and dynamically adjustable, when the composite magnetic material is applied to the electronic equipment, the electronic equipment can be protected from the influence of external electromagnetic interference, so that the compatible use of the electronic equipment in a high-frequency environment and a low-frequency environment is realized, and in addition, the adaptive composite magnetic material can be selected according to the characteristics of different electronic equipment and can be applied to specific scenes.
Hereinafter, the composite magnetic material, the method of preparing the same and the application thereof will be further described by the following specific examples.
Example 1
Under the protection of inert gas, respectively mixing and heating a mixture of metal simple substances with Fe 2O3、Mn3O4 and ZnO, niO, mgO, wherein when the metal simple substances are selected from zinc, iron, magnesium, manganese or nickel, the mass ratio of zinc to Fe 2O3、Mn3O4 and ZnO, niO, mgO is 4.5:0:1:1:1:1, the heating temperature is 900 ℃, the heating time is 1.5 hours, when the metal simple substances are selected from iron, the mass ratio of iron to Fe 2O3、Mn3O4 and ZnO, niO, mgO is 5:0.5:1:1, the heating temperature is 1450 ℃, the heating time is 2.5 hours, the mass ratio of magnesium to Fe 2O3、Mn3O4 and ZnO, niO, mgO is 4:0.5:1:1:1:1, the heating temperature is 1000 ℃, the mass ratio of manganese to Fe 2O3、Mn3O4 and ZnO, niO, mgO is 3:1:1:1:1, the heating time is 1200 ℃, the heating time is 3 hours, the mass ratio of the metal simple substances is selected from nickel and the heating time is 2.5:1:1, the mass ratio of magnesium to Fe 2O3、Mn3O4 and ZnO, niO, mgO is 4:0.5:1:1:1, the heating time is 1000 ℃, and the heating time is 1:1:1:1:6:3:1; and then adding silicon into the heated product respectively, wherein the mass ratio of the metal simple substance to the silicon is 15:1, and solidifying at 20-40 ℃ to obtain a solidified product.
Respectively crushing the obtained solidification products to obtain crushed products, respectively cleaning the obtained crushed products with hydrogen peroxide solution with the concentration of 8.1 mol/L to remove impurities, and then cleaning with ammonia water with the mass fraction of 20% to remove residual hydrogen peroxide solution on the surface of the crushed products, wherein the particle size of the zinc-based crushed products is 550nm-650nm, the particle size of the iron-based crushed products is 650nm-850nm, the particle size of the magnesium-based crushed products is 850nm-1050nm, the particle size of the manganese-based crushed products is 1100nm-1300nm, and the particle size of the nickel-based crushed products is 1300nm-1500nm. Layering the crushed product by adopting a leaching method, and then drying to obtain a magnetic powder raw material, wherein the particle size of the zinc-based magnetic powder raw material is 600nm plus or minus 50nm, the particle size of the iron-based magnetic powder raw material is 775nm plus or minus 75nm, the particle size of the magnesium-based magnetic powder raw material is 950nm plus or minus 50nm, the particle size of the manganese-based magnetic powder raw material is 1250nm plus or minus 50nm, and the particle size of the nickel-based magnetic powder raw material is 1350nm plus or minus 50nm.
The method comprises the steps of magnetizing a magnetic powder raw material in an electromagnetic environment to obtain composite magnetic powder, wherein the magnetic field intensity is 100 gauss in the process of magnetizing the zinc-based magnetic powder raw material, the magnetic permeability of the zinc-based composite magnetic powder is 750, the magnetic field intensity is 145 gauss in the process of magnetizing the iron-based magnetic powder raw material, the magnetic permeability of the iron-based composite magnetic powder is 1300, the high-power scanning electron microscope image of the iron-based composite magnetic powder is shown in fig. 1, the magnetic field intensity is 60 gauss in the process of magnetizing the magnesium-based magnetic powder raw material, the magnetic permeability of the magnesium-based composite magnetic powder is 1800, the magnetic field intensity is 75 gauss in the process of magnetizing the manganese-based magnetic powder raw material, the magnetic permeability of the manganese-based composite magnetic powder is 2300, the magnetic field intensity of the nickel-based composite magnetic powder raw material is 125 gauss, and the magnetic permeability of the nickel-based composite magnetic powder is 3400.
Under the protection of inert gas, the ferric oxide is pressurized and heated to obtain a heated product, wherein the pressure is increased to 50kPa from 5kPa, the speed is increased to 1kPa/5min, the temperature is 250 ℃, and the time is 1 hour.
And applying a mist silica gel to the heated product, wherein the mass ratio of the heated product to the mist is 12:1.
Magnetizing the skeleton, wherein the magnetic field intensity is increased from the center of the skeleton to the edge, specifically, the magnetic field intensity of the center of the skeleton is 40 gauss, the magnetic field intensity of the edge is 180 gauss, the ferromagnetic oxide skeleton is obtained, the magnetic field intensity of the center of the ferromagnetic oxide skeleton is 35 gauss, the magnetic field intensity of the edge is 175 gauss, and the aperture of the magnetic skeleton is 6-8 mu m.
Mixing the iron oxide magnetic skeleton with zinc-based composite magnetic powder, iron-based composite magnetic powder, magnesium-based composite magnetic powder, manganese-based composite magnetic powder and nickel-based composite magnetic powder in sequence, and carrying out magnetic vibration, wherein the mass ratio of the iron oxide magnetic skeleton to the zinc-based composite magnetic powder to the iron-based composite magnetic powder to the magnesium-based composite magnetic powder to the manganese-based composite magnetic powder to the nickel-based composite magnetic powder is 15:2:1.5:1.5:1:1, so as to obtain the composite magnetic material, and the mass ratio of the magnetic skeleton to the composite magnetic powder is 2:1, wherein a high-power scanning electron microscope image of the composite magnetic material is shown in figure 2.
Comparative example 1
Comparative example 1 was conducted with reference to example 1, except that only an iron-based composite magnetic powder was mixed with an iron oxide magnetic skeleton and magnetically vibrated, the amount of the iron-based composite magnetic powder being the total mass of the iron-based composite magnetic powder, zinc-based composite magnetic powder, nickel-based composite magnetic powder, manganese-based composite magnetic powder, magnesium-based composite magnetic powder in example 1.
Comparative example 2
Comparative example 2 was conducted with reference to example 1, except that only magnesium-based composite magnetic powder was mixed with the iron oxide magnetic skeleton and magnetically vibrated, the amount of the magnesium-based composite magnetic powder being the total mass of the iron-based composite magnetic powder, the zinc-based composite magnetic powder, the nickel-based composite magnetic powder, the manganese-based composite magnetic powder, and the magnesium-based composite magnetic powder in example 1.
Comparative example 3
Comparative example 3 was performed with reference to example 1, except that zinc-based composite magnetic powder, iron-based composite magnetic powder, manganese-based composite magnetic powder, magnesium-based composite magnetic powder, nickel-based composite magnetic powder were mixed first, and then the resultant mixture was mixed with an iron oxide magnetic skeleton and magnetically vibrated.
Comparative example 4
Comparative example 4 referring to example 1, except that the order of adding the composite magnetic powder to the iron oxide magnetic skeleton was adjusted, the order of adding the composite magnetic powder was zinc-based composite magnetic powder, iron-based composite magnetic powder, manganese-based composite magnetic powder, magnesium-based composite magnetic powder, nickel-based composite magnetic powder.
Comparative example 5
Comparative example 5 was performed with reference to example 1, except that an iron-oxide magnetic skeleton was sequentially mixed with an iron-based composite magnetic powder and a magnesium-based composite magnetic powder, and magnetic vibration was performed, wherein the total amount of the iron-based composite magnetic powder and the magnesium-based composite magnetic powder was the total mass of the iron-based composite magnetic powder, the zinc-based composite magnetic powder, the nickel-based composite magnetic powder, the manganese-based composite magnetic powder, and the magnesium-based composite magnetic powder in example 1, and the mass ratio of the iron-based composite magnetic powder to the magnesium-based composite magnetic powder was 1:1.
Test example 1
The magnetic properties of the composite magnetic materials obtained in example 1 and comparative examples 1 to 5 were tested as shown below, the test results are shown in table 1, and the magnetic permeability versus frequency of the composite magnetic material obtained in example 1 is shown in fig. 3, and it can be seen from fig. 3 that the composite magnetic material has a high magnetic permeability in the frequency range of 1kHz to 1GHz, and in fig. 3, μ' represents the real magnetic permeability and μ″ represents the imaginary magnetic permeability.
And (3) testing the magnetic focusing performance, namely referring to JB/T13536-2018, focusing the magnetic focusing frequency band with the magnetic permeability of more than 1000, and testing the magnetic permeability of the composite magnetic material in the focusing magnetic frequency band.
Wave absorbing performance test insertion loss was tested with reference to GB/T32596.
TABLE 1
Example 2
Example 2 was performed with reference to example 1, except that the mass ratio of zinc-based composite magnetic powder, iron-based composite magnetic powder, magnesium-based composite magnetic powder, manganese-based composite magnetic powder, nickel-based composite magnetic powder was 1:1:1:1.5.
Example 3
Example 3 was performed with reference to example 1, except that the mass ratio of zinc-based composite magnetic powder, iron-based composite magnetic powder, magnesium-based composite magnetic powder, manganese-based composite magnetic powder, nickel-based composite magnetic powder was 1:1.5:1:1.
Example 4
Example 4 was performed with reference to example 1, except that in the step of pressurizing and heating the iron oxide, the temperature was 200 ℃.
Example 5
Example 5 was performed with reference to example 1, except that in the step of pressurizing and heating the iron oxide, the temperature was 300 ℃.
Example 6
Example 6 was performed with reference to example 1, except that the magnetic field strength was 90 gauss during the magnetizing of the zinc-based magnetic powder raw material, the magnetic permeability of the zinc-based composite magnetic powder was 600, the magnetic field strength was 140 gauss during the magnetizing of the iron-based magnetic powder raw material, the magnetic permeability of the iron-based composite magnetic powder was 1200, the magnetic field strength was 50 gauss during the magnetizing of the magnesium-based magnetic powder raw material, the magnetic permeability of the magnesium-based composite magnetic powder was 1500, the magnetic field strength was 70 gauss during the magnetizing of the manganese-based magnetic powder raw material, the magnetic permeability of the manganese-based composite magnetic powder was 2100, the magnetic field strength was 120 gauss during the magnetizing of the nickel-based magnetic powder raw material, and the magnetic permeability of the nickel-based composite magnetic powder was 2500.
Example 7
Example 7 was performed with reference to example 1, except that the magnetic field strength was 110 gauss during the magnetizing of the zinc-based magnetic powder raw material, the magnetic permeability of the zinc-based composite magnetic powder was 800, the magnetic field strength was 150 gauss during the magnetizing of the iron-based magnetic powder raw material, the magnetic permeability of the iron-based composite magnetic powder was 1300, the magnetic field strength was 65, the magnetic permeability of the magnesium-based composite magnetic powder was 1900 during the magnetizing of the manganese-based magnetic powder raw material, the magnetic field strength was 80, the magnetic permeability of the manganese-based composite magnetic powder was 2200, the magnetic field strength was 130, and the magnetic permeability of the nickel-based composite magnetic powder was 3200 during the magnetizing of the nickel-based magnetic powder raw material.
Example 8
Example 8 the procedure of example 1 was carried out, except that the particle size of the zinc-based magnetic powder raw material was 550 nm.+ -.50 nm, the particle size of the iron-based magnetic powder raw material was 650 nm.+ -.50 nm, the particle size of the magnesium-based magnetic powder raw material was 850 nm.+ -.50 nm, the particle size of the manganese-based magnetic powder raw material was 1050 nm.+ -.50 nm, and the particle size of the nickel-based magnetic powder raw material was 1250 nm.+ -.50 nm.
Example 9
Example 9 was conducted with reference to example 1, except that the particle size of the zinc-based magnetic powder raw material was 650 nm.+ -.50 nm, the particle size of the iron-based magnetic powder raw material was 850 nm.+ -.50 nm, the particle size of the magnesium-based magnetic powder raw material was 1050 nm.+ -.50 nm, the particle size of the manganese-based magnetic powder raw material was 1250 nm.+ -.50 nm, and the particle size of the nickel-based magnetic powder raw material was 1450 nm.+ -.50 nm.
Example 10
Example 10 was conducted with reference to example 1, except that the magnetic permeability of the composite magnetic powder was gradually reduced in stages in the direction from the center to the edge of the magnetic skeleton, specifically, the particle diameter of the nickel-based composite magnetic powder was 600nm±50nm, the particle diameter of the manganese-based composite magnetic powder was 775nm±75nm, the particle diameter of the magnesium-based composite magnetic powder was 950nm±50nm, the particle diameter of the iron-based composite magnetic powder was 1250nm±50nm, and the particle diameter of the zinc-based composite magnetic powder was 1350 nm. Meanwhile, the iron oxide magnetic skeleton is sequentially mixed with nickel-based composite magnetic powder, manganese-based composite magnetic powder, magnesium-based composite magnetic powder, iron-based composite magnetic powder and zinc-based composite magnetic powder and subjected to magnetic vibration to obtain the composite magnetic material.
Test example 2
The magnetic properties of the composite magnetic materials obtained in examples 2 to 10 were measured with reference to test example 1, and the test results are shown in table 2.
TABLE 2
Example 11
Example 11 was conducted with reference to example 1, except that the iron-oxide magnetic skeleton was mixed with the iron-based composite magnetic powder, the magnesium-based composite magnetic powder, and the nickel-based composite magnetic powder in this order, and magnetic vibration was performed, and in the composite magnetic material, the iron-based composite magnetic powder, the magnesium-based composite magnetic powder, and the nickel-based composite magnetic powder were sequentially filled in the magnetic skeleton in a direction from the center to the edge of the magnetic skeleton.
Example 12
Example 12 was conducted with reference to example 1, except that the iron oxide magnetic skeleton was mixed with zinc-based composite magnetic powder, manganese-based composite magnetic powder, nickel-based composite magnetic powder in this order, and magnetic vibration was applied to the composite magnetic material in which zinc-based composite magnetic powder, manganese-based composite magnetic powder, nickel-based composite magnetic powder were filled in this order in the direction from the center to the edge of the magnetic skeleton.
Example 13
Example 13 was conducted with reference to example 10, except that the iron oxide magnetic skeleton was mixed with nickel-based composite magnetic powder, manganese-based composite magnetic powder, iron-based composite magnetic powder in this order, and magnetic vibration was applied to the composite magnetic material in which the nickel-based composite magnetic powder, manganese-based composite magnetic powder, iron-based composite magnetic powder were filled in this order in the direction from the center to the edge of the magnetic skeleton.
Example 14
Example 14 was conducted with reference to example 10, except that the iron oxide magnetic skeleton was mixed with the manganese-based composite magnetic powder, the magnesium-based composite magnetic powder, and the iron-based composite magnetic powder in this order, and magnetic vibration was performed, and in the composite magnetic material, the manganese-based composite magnetic powder, the magnesium-based composite magnetic powder, and the iron-based composite magnetic powder were sequentially filled in the magnetic skeleton in the direction from the center to the edge of the magnetic skeleton.
Test example 3
The magnetic properties of the composite magnetic materials obtained in examples 11 to 14 were measured with reference to test example 1, and the test results are shown in table 3.
TABLE 3 Table 3
The technical features of the above embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
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