CN113643893A - Soft magnetic composite material and preparation method thereof - Google Patents

Soft magnetic composite material and preparation method thereof Download PDF

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CN113643893A
CN113643893A CN202110981631.6A CN202110981631A CN113643893A CN 113643893 A CN113643893 A CN 113643893A CN 202110981631 A CN202110981631 A CN 202110981631A CN 113643893 A CN113643893 A CN 113643893A
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soft magnetic
easy
magnetic powder
magnetic material
powder
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王涛
王国武
汪小明
郭春生
乔亮
李发伸
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Guangzhou Xinlaifu New Material Co ltd
Lanzhou University
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Guangzhou Xinlaifu New Material Co ltd
Lanzhou University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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 for manufacturing cores, coils, or magnets
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147Alloys characterised by their composition
    • H01F1/14708Fe-Ni based alloys
    • H01F1/14733Fe-Ni based alloys in the form of particles

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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

The invention relates to a soft magnetic composite material and a preparation method thereof. A method for preparing a soft magnetic composite material comprising: preparing the easy-to-surface magnetic powder of the soft magnetic composite material; preparing the flour-susceptible magnetic powder and the binding material into mixed slurry according to a preset proportion; orienting the easy-to-magnetize surfaces of the easy-to-magnetize magnetic powder in the mixed slurry to be parallel arrangement in an external magnetic field; the mixed slurry is dried and hot-pressed to make a soft magnetic composite material. The preparation of the easy-to-surface magnetic powder may include preparing microparticles of a soft magnetic material, performing heat treatment to relieve stress, performing ball milling treatment to prepare the easy-to-surface magnetic powder, and performing washing, filtering, and drying. The preparing of the easy-to-surface magnetic powder may also include depositing a sacrificial layer on the substrate, depositing a soft magnetic material layer on the sacrificial layer, etching the soft magnetic material layer to divide into a plurality of regions of a desired size, removing the sacrificial layer to peel off the soft magnetic material layer, obtaining the easy-to-surface magnetic powder, and washing, filtering, and drying the easy-to-surface magnetic powder.

Description

Soft magnetic composite material and preparation method thereof
Technical Field
The present invention generally relates to the field of high frequency soft magnetic materials, and more particularly, to a high frequency soft magnetic material that can be used for electromagnetic energy and signal transmission and conversion applications in a frequency band above mhz, and a method for preparing the same.
Background
The high-frequency soft magnetic material is an important basic material indispensable to electronic equipment in the fields of electric power, communication and the like, and has the function of converting and adjusting 'coarse electricity' acquired from a power generation device into 'fine electricity' suitable for user electronic equipment. With the development and popularization of the field of intelligent terminals, new energy vehicles, portable electronic devices, 5G equipment and the like, electronic equipment is developing towards the direction of higher work efficiency, lower loss and miniaturization so as to meet the requirements of technical development and energy conservation and consumption reduction in the related field. At present, it is considered that the high frequency is the most effective way to improve the operating efficiency of electronic equipment and reduce the loss. The advent of the third generation Wide Bandgap (WBG) semiconductor has enabled the operating frequency of power supply devices to be increased to higher frequencies, providing further opportunities for implementing higher frequency electronic devices. However, as essential basic materials for electronic devices, none of the currently commercially available soft magnetic materials can effectively operate in this higher frequency band.
According to Snoek's law, for the soft magnetic materials widely used at present, the Snoek product [ (mu ] isi-1)·fr]Is a constant value, where μiTo initial permeability, frIs the natural resonant frequency (or referred to as the cut-off frequency). That is, with the operating frequency frIncrease of magnetic permeability mu of soft magnetic materialiIt will drop significantly making it ineffective at high frequency bands. Therefore, the conventional soft magnetic material has not been satisfactory for the third generation semiconductorThe mating requirements of the bulk device.
The applicant provides a two-dimensional magnetic moment soft magnetic composite material in an invention patent 201910000894.7, which can break through the Snoek limit and meet the requirement of high-frequency application by orienting the magnetic moment of micro powder in a two-dimensional plane and orienting the two-dimensional magnetic moment micro powder dispersed in an insulating matrix to distribute the magnetic moment in the two-dimensional plane. However, such new materials present new challenges to the manufacturing process. It would be desirable to have a process that efficiently produces soft magnetic composite materials that meet the above requirements and is suitable for industrial mass production.
Disclosure of Invention
The high-frequency soft magnetic composite material provided by the invention comprises easy-to-surface soft magnetic material micro powder, such as easy-to-surface magnetic powder of FeNi material, the easy magnetization direction of the easy-to-surface soft magnetic material is in the lamellar plane of the easy-to-surface magnetic powder, and the plane orientation degree of magnetic moment in the magnetic powder can reach more than 95%. As the easy magnetization axes of the soft magnetic material are only distributed in a specific plane, the Snoek limit can be broken through, and higher magnetic permeability is obtained at high frequency. In the soft magnetic composite material made of the easy-to-surface magnetic powder, the easy-to-magnetize surfaces of the easy-to-surface magnetic powder are arranged in parallel along the plane of an external orientation magnetic field, so that the effective working frequency of more than 30MHz and higher magnetic permeability can be obtained in the final bulk composite material along the plane. The manufacturing method of the invention can efficiently prepare the easy-to-surface magnetic powder, thus being very suitable for the industrialized large-scale production of the soft magnetic composite material for high-frequency electronic devices.
According to an embodiment, there is provided a method of preparing a soft magnetic composite material, comprising: preparing easy-to-surface magnetic powder of a soft magnetic material, wherein the magnetic powder has an easy-to-magnetize surface; preparing the easy-to-surface magnetic powder of the soft magnetic composite material and the binding material into mixed slurry according to a preset proportion; orienting easy-to-magnetize surfaces of the easy-to-surface magnetic powder in the mixed slurry to be arranged in parallel along the external magnetic field; and drying and hot-pressing the mixed slurry oriented by the external magnetic field to prepare the soft magnetic composite material. Wherein, preparing the easy-to-surface magnetic powder of the soft magnetic composite material can comprise: preparing microparticles of a soft magnetic material; heat-treating the microparticles of the soft magnetic material to relieve stress; carrying out ball milling treatment on the microparticles of the soft magnetic material to prepare the easy-to-wear magnetic powder; and washing, filtering and drying the easy-to-surface magnetic powder of the soft magnetic material. Alternatively, preparing the easy-to-surface magnetic powder of a soft magnetic material may include: depositing a sacrificial layer on a substrate; depositing a soft magnetic material layer on the sacrificial layer; etching the soft magnetic material layer to divide it into a plurality of regions having desired sizes; removing the sacrificial layer to strip the soft magnetic material layer from the substrate to obtain easy-surface magnetic powder of the soft magnetic material; and washing, filtering and drying the easy-to-surface magnetic powder of the soft magnetic material.
In some embodiments, the soft magnetic material is Fe1-xNixAnd x is in the range of 0.35 to 0.9.
In some embodiments, the degree of planar orientation of magnetic moments within the easy-to-surface magnetic powder of the soft magnetic material in the soft magnetic composite material is greater than 95%.
In some embodiments, the soft magnetic material has an easy-to-surface magnetic powder having a diameter-thickness ratio of 40 to 150.
In some embodiments, the bonding material comprises one or more of polyurethane, epoxy, polyimide.
In some embodiments, in the mixed slurry, the easy-surface magnetic powder of the soft magnetic material accounts for 30% to 65% of the total volume of the easy-surface magnetic powder of the soft magnetic material and the binder material.
In some embodiments, the microparticles of soft magnetic material have a particle size of 10-50 μm.
In some embodiments, the heat treatment temperature at which the fine particles of the soft magnetic material are heat-treated is in a range of 250 ℃ to 500 ℃.
In some embodiments, the sacrificial layer comprises an aluminum layer, and removing the sacrificial layer comprises etching the aluminum layer with an alkaline solution. The alkali solution comprises one or more of a sodium hydroxide solution and a potassium hydroxide solution.
In some embodiments, the mixed slurry is subjected to a drying process while the external magnetic field is applied to the mixed slurry to align the easy-to-magnetize faces of the easy-to-face magnetic powder in parallel.
In some embodiments, subjecting the dried mixed slurry to a hot pressing process includes pressing in a direction perpendicular to the easy-to-magnetize face of the easy-to-face magnetic powder.
According to another embodiment, there is provided a soft magnetic composite material prepared by any one of the above methods.
According to another embodiment, an electronic device is provided, comprising an insulated magnetic component made of the above soft magnetic composite material.
The above and other features and advantages of the present invention will become apparent from the following description of specific embodiments, which is to be read in connection with the accompanying drawings.
Drawings
Fig. 1 shows a flow chart of a method for preparing a soft magnetic composite material according to an embodiment of the present invention.
Fig. 2 shows a flow chart of a method for producing an easy-to-surface magnetic powder of a soft magnetic material according to an embodiment of the invention.
Fig. 3 shows a flow chart of a method for producing an easy-to-surface magnetic powder of a soft magnetic material according to another embodiment of the invention.
FIG. 4 shows a schematic diagram of an orientation operation using an external magnetic field, according to an embodiment of the invention.
Fig. 5 shows a micrograph of a soft magnetic composite material prepared according to an embodiment of the present invention.
Fig. 6 shows hysteresis curves of soft magnetic composite materials prepared according to an embodiment of the present invention in different directions.
Fig. 7 shows a graph of the complex permeability spectrum of the soft magnetic composite material prepared according to an embodiment of the present invention.
Fig. 8 shows a graph of the complex permeability spectrum of a soft magnetic composite material prepared according to another embodiment of the present invention.
Detailed Description
Hereinafter, example embodiments according to the present application will be described in detail with reference to the accompanying drawings. Note that the drawings may not be to scale. It should be apparent that the described embodiments are merely some embodiments of the present application and not all embodiments of the present application, which are not limited to the example embodiments described herein.
Fig. 1 shows a flow chart of a method for preparing a soft magnetic composite material according to an embodiment of the present invention. In the method, the easy-to-surface magnetic powder of soft magnetic materials such as FeNi can be prepared, so that the easy magnetization direction of the easy-to-surface magnetic powder is in the lamellar plane of the magnetic powder, and the plane orientation degree of the magnetic moment in the magnetic powder can reach more than 95 percent, thereby obtaining the easy-to-surface magnetic powder. Further, in the process of preparing a soft magnetic composite material using such an easy-to-surface magnetic powder, easy-to-surface magnetic powders are arranged in parallel with each other by a rotating magnetic field, and then subjected to drying and hot-pressing treatment, so that the easy-to-surface magnetic powders can be fixed in the parallel plane in the resulting soft magnetic composite material. The manufacturing method of the invention can efficiently prepare the easy-to-surface magnetic powder, and the plane orientation degree of the magnetic moment in the easy-to-surface magnetic powder in the prepared soft magnetic composite material can reach more than 95 percent, and the material can realize the effective working frequency of more than 30MHz and higher magnetic conductivity. Therefore, the method of the present invention is very suitable for the industrial mass production of soft magnetic composite materials for high frequency electronic devices. It should be understood that although the embodiments of the present invention are described herein with FeNi as an example, this is merely to enable one skilled in the art to practice the embodiments taught herein, and that the techniques and methods of the present invention may also be applied to the preparation of other soft magnetic materials such as carbonyl iron, FeSi, FeCo, FeSiAl, FeNiMo, and the like, for example, for easy-facing magnetic powders.
A method 100 of preparing a soft magnetic composite material according to an embodiment of the present invention is described in detail below with reference to fig. 1. Referring to fig. 1, in step 110, an easy-to-surface magnetic powder of a soft magnetic material may be prepared. The soft magnetic material may be, for example, Fe1-xNixWherein x may be in the range of 0.35 to 0.9. Fig. 2 shows a flow diagram of a method 200 for producing an easy-to-surface magnetic powder of a soft magnetic material according to an embodiment of the invention. Referring to fig. 2, in step 210, microparticles of a soft magnetic material, such as FeNi, may be prepared using a water atomization process or an air atomization process, and the particles may have a substantially spherical shape, and a diameter thereof may be, for example, in the range of 5-50 μm, preferably in the range of 10-30 μm. It should be understood that when preparing the easy-to-wear magnetic powder or microparticles in the method of the present invention, it is not the easy-to-prepare powderThe magnetic flour or microparticles all fall within the shape parameters described herein, but a majority, e.g., more than 80%, preferably more than 90%, of them fall within the shape parameters described herein.
At step 220, the microparticles of soft magnetic material may be heat treated (thermally annealed) to relieve stress therein. The microparticles of the soft magnetic material may be heated to a predetermined annealing temperature in a vacuum environment or a low-pressure environment protected by an inert gas such as an inert gas, held for a predetermined time, and then slowly cooled, for example, naturally cooled to room temperature. For soft magnetic metal or alloy materials, the annealing temperature may generally be in the range of 250 ℃ to 500 ℃, for example for FeNi the annealing temperature may be in the range of 350 ℃ to 450 ℃. The incubation time may typically be in the range of 10 minutes to 6 hours, for example typically in the range of 30 minutes to 2 hours. Through annealing treatment, the uniformity of a metal structure can be improved, residual stress in the microparticles is eliminated, and the plasticity and the toughness of the microparticles are improved. The inventor finds that the stress-relief thermal annealing treatment is very beneficial to the subsequent ball milling (or sanding) process, which helps to obtain the easy-to-surface magnetic powder with high planar orientation degree through the ball milling treatment, and reduces the proportion of material scrap powder generated in the ball milling process, thereby improving the yield of the easy-to-surface magnetic powder.
Next, in step 230, the soft magnetic material particles after stress relief annealing may be ball-milled to prepare the easy-to-surface magnetic powder. Ball milling can be performed by selecting steel balls of an appropriate size and adding a commonly used dispersant or surfactant, such as stearic acid, polyethylene glycol, or the like. The ball milling may be generally performed in a plurality of stages, for example, after a predetermined time of ball milling, the ball milling may be supplemented with a dispersant or a surfactant, and then continued. The ball milling time is generally in the range of 1 to 8 hours. In the time range, the soft magnetic material micro-particles become thinner under the impact of the steel ball, and the easy-to-surface magnetic powder with the expected diameter-thickness ratio is formed. If the ball milling time is longer, too small a crumb soft magnetic micropowder tends to exhibit superparamagnetism, which is also undesirable.
After the ball milling process is performed, the obtained easy-to-surface magnetic powder may be washed and filtered at step 240. The magnetic powder of the easy-to-surface material can be washed for many times, for example, alcohol, acetone, deionized water and the like are used for washing for many times, and the filtering is carried out to filter impurities and some tiny fragments of the soft magnetic material, so that the magnetic powder of the soft magnetic material with uniform size and diameter-thickness ratio mainly in the range of 40-150 is obtained. The easy-to-surface magnetic powder of the soft magnetic material may then be dried, for example by baking or air drying, for later use in the manufacture of soft magnetic composites.
The method shown in fig. 2 is well suited for cubic system soft magnetic materials such as FeNi, CoFe, etc., and the X and Y axis directions (in the sheet plane) of the easy-to-surface magnetic powder obtained by ball milling have extremely low shape anisotropy properties as compared with the Z axis direction (in the sheet normal direction), so that the easy magnetization axis is easily oriented into the X-Y plane.
Another embodiment also provides a method of producing a magnetic easy-to-roll powder having more uniform size and thickness, which is illustrated in fig. 3. Referring to fig. 3, a method 300 of preparing an easy-to-surface magnetic powder of soft magnetic material may begin by depositing a sacrificial layer on a substrate, such as a silicon wafer, at step 310. Here, the sacrificial layer is a material on which a soft magnetic material layer can be deposited and easily removed, for example, an Al layer may be used, and its deposition method may include magnetron sputtering, pulsed laser deposition, or the like, and its thickness may be in the range of 10nm to 200nm, preferably in the range of 50nm to 150 nm.
Next, at step 320, a soft magnetic material layer may be deposited on the sacrificial layer, such as a FeNi soft magnetic material layer deposited on an Al sacrificial layer. Magnetron sputtering or pulsed laser deposition or the like may also be used to deposit the soft magnetic material layer. The thickness of the soft magnetic material layer may be in the range of 100nm to 1 μm, for example, may be around 500 nm.
In step 330, the soft magnetic material layer may be etched into a plurality of regions of desired dimensions. Ion beam etching may be used to etch the sacrificial layer and the soft magnetic material layer. For example, a photoresist pattern may be first formed on the soft magnetic material layer using a photolithography process, and then the soft magnetic material layer and the sacrificial layer thereunder may be etched using the photoresist pattern as a mask. Using the photoresist pattern, the soft magnetic material layer may be etched into a plurality of regions of desired shape and size, for example, circular regions having a diameter of 1 μm to 200 μm.
Next, in step 340, the sacrificial layer may be removed to exfoliate the soft magnetic material layer to obtain an easy-to-surface magnetic powder of the soft magnetic material. Chemical solvents may be used to remove the sacrificial layer, for example, using an alkaline solution such as NaOH or KOH solution to etch away the Al sacrificial layer.
The resultant soft magnetic material easy-to-surface magnetic powder may then be washed and filtered to remove impurities or debris to obtain soft magnetic material easy-to-surface magnetic powder of relatively uniform size at step 350. The easy-to-surface magnetic powder of the soft magnetic material may then be dried, for example by baking or air drying, for later use in the manufacture of soft magnetic composites.
The process steps for preparing the easy-to-noodle magnetic powder are described above. Referring back to fig. 1, in step 120, the easy-to-surface magnetic powder and the binding material may be added to a solvent, such as acetone or alcohol, according to a predetermined ratio to prepare a mixed slurry. The binding material can be organic insulating binding material such as polyurethane, epoxy resin, polyimide and the like, and the volume ratio of the easy-surface magnetic powder only accounts for 30-65% of the total volume of the easy-surface magnetic powder and the binding material of the soft magnetic composite material. The flour-susceptible magnetic powder can be sufficiently and uniformly dispersed in the mixed slurry by stirring, ultrasonic treatment and the like.
In step 130, the easy magnetization plane of the easy-plane magnetic powder in the mixed slurry may be oriented to be aligned parallel to the plane of the external magnetic field using the external magnetic field. The magnetic field orientation step can be performed by subjecting the mixed slurry to an external magnetic field after ultrasonication, stirring, or air drying to a desired viscosity. Fig. 4 shows an example of using a rotating magnetic field, the mixed slurry can be placed between two magnetic poles S (south pole) and N (north pole), which can rotate around the mixed slurry. In some embodiments, pairs of poles may also be disposed around the mixed slurry. Under the action of the magnetic field, the easy-to-surface magnetic powder in the mixed slurry can be oriented to be arranged in parallel with the plane of the external magnetic field, so that the easy-to-magnetization surfaces in all the magnetic powder are parallel to each other. By making the mixed slurry have appropriate viscosity, the easy-to-wear magnetic powder can be rotated to the oriented direction. Or in some embodiments, the mixed slurry may be simultaneously subjected to a drying process, such as drying or airing, during the orientation process using the external magnetic field, to gradually increase its viscosity. Thus, in the initial stage of orientation treatment, the mixed slurry has low viscosity, so that the easy-to-surface magnetic powder of the soft magnetic material can be easily oriented to the parallel direction by an external magnetic field through the rotation of the magnetic powder; as the orientation treatment proceeds, the viscosity of the mixed slurry gradually increases, so that the easy-to-surface magnetic powder of the soft magnetic material can be easily held in the oriented parallel direction.
Next, in step 140, the mixed slurry may be subjected to drying and hot pressing to make a soft magnetic composite material. Drying or airing can be carried out, and then hot pressing is carried out. When hot pressing is carried out, the mixed material can be heated to the softening temperature of the binding material, and meanwhile, pressure is applied in the direction vertical to the easy magnetization surface of the easy-to-surface magnetic powder of the soft magnetic material, so that the mixed material is pressed into the block soft magnetic composite material with high density. Because the extrusion is carried out in the direction vertical to the easy-magnetization surface, the easy-surface magnetic powder in the obtained soft magnetic composite material can still keep parallel orientation, and can not be bent due to extrusion so as to be oriented to the direction vertical to the normal (namely the Z-axis direction).
By the method, the easy-to-surface soft magnetic composite material can be prepared, and high magnetic moment plane orientation degree can be obtained, so that the method can be suitable for application in high-frequency electronic devices. Fig. 5 shows a micrograph of a sample of a soft magnetic composite prepared according to the above method, wherein the right image is a higher resolution photograph of the square portion in the left image. As can be seen from fig. 5, all the micropowder is aligned neatly and in parallel in the composite material by magnetic orientation, showing a distinct orientation texture.
FIG. 6 is a magnetic hysteresis loop of a sample of a soft magnetic composite material in which FeNi easy-surface magnetic powder and polyurethane are mixed in a volume ratio of 1:1 and a block sample having a diameter-thickness ratio of 1:1 is prepared, and the magnetic hysteresis loops in directions of X, Y and a Z-axis are measured, respectively, wherein an X-Y plane is a plane in which a rotating magnetic field of the soft magnetic composite material is oriented and the Z-axis is a vertical normal direction. As can be seen from fig. 6, the sample was easily saturated in magnetization in the X and Y axis directions, and the hysteresis loops in both directions almost completely overlapped, which indicates that the composite formed an easy magnetization plane along the orientation plane, and that the composite exhibited low magnetic anisotropy in the orientation plane. In the Z-axis direction, the sample is hard to be magnetized and saturated because the Z-axis direction is the hard-axis direction, and thus it is difficult for the external magnetic field to deflect the magnetic moment in the soft magnetic material easy-surface magnetic powder to the hard-axis direction.
TABLE 1
Figure BDA0003229334080000071
Table 1 above shows the static magnetic parameters for each direction, including saturation magnetization Ms, remanence Mr, and coercivity Hc. Here, the remanence Mr in the out-of-plane direction comes from the magnetic moment vector of the fine powder of the soft magnetic material which is not completely oriented along the orientation plane. From the ratio of this value to the total magnetization, the Degree of Planar Orientation (DPO) of the magnetic moment of the composite material can be estimated, which is represented by the following equation 1.
Figure BDA0003229334080000081
Where Mr (Z-axis) is the remanence in the Z-axis direction. From equation 1 and the magnetic parameters shown in table 1, it can be estimated that the degree of plane orientation of the magnetic moment of the sample is about 99.0%.
Fig. 7 shows a graph of the complex permeability spectrum of the soft magnetic composite sample prepared according to the method shown in fig. 1 and 2. The sample is made of a FeNi soft magnetic material, and the volume ratio of FeNi easy-surface magnetic powder to polyurethane is 1: 1. The values of the real and imaginary μ' and μ "permeability at the relevant fixed frequency points are shown in table 2 below. As shown in the figure and the following table, the composite material shows the real part and the imaginary part of the magnetic permeability which hardly changes with the frequency within 30MHz, wherein the real part mu 'is about 37, and the imaginary part mu' is less than 1, which indicates that the effective use frequency band of the soft magnetic composite material can reach 30 MHz.
TABLE 2
1MHz 10MHz 20MHz 30MHz 50MHz 100MHz 1GHz
Real part mu' 37.3 37.2 37.3 37.8 39.0 40.0 22.2
Imaginary part mu' 0 0.2 0.4 0.8 2.4 7.1 17.5
Fig. 8 is a graph showing a complex permeability spectrum of a soft magnetic composite material prepared according to the method shown in fig. 1 and 3. The sample adopts an Al sacrificial layer with the thickness of 100nm and a FeNi soft magnetic material layer with the thickness of 500nm, the soft magnetic material layer is etched by ion beams to obtain a wafer with the diameter of 20 mu m, and the Al sacrificial layer is corroded by NaOH solution to obtain the easy-to-surface magnetic powder. The FeNi easy-surface magnetic powder and polyurethane are prepared into a soft magnetic composite material sample according to the volume ratio of 3: 7. The values of the real and imaginary μ' and μ "permeability at the relevant fixed frequency points are shown in table 3 below. As shown in the figure and the following table, the composite material shows the real part and the imaginary part of the magnetic permeability which hardly changes with the frequency within 50MHz, wherein the real part mu 'is about 16.7, and the imaginary part mu' is less than 1, which indicates that the effective using frequency band of the soft magnetic composite material can reach 50 MHz.
TABLE 3
1MHz 10MHz 20MHz 30MHz 50MHz 100MHz 1GHz
Real part mu' 16.9 16.6 16.7 16.7 16.9 17.4 9.4
Imaginary part mu' 0 0 0 0.1 0.1 1.4 7.3
Soft magnetic composites and methods of making soft magnetic composites according to some embodiments of the present invention are described above. It will be appreciated that the soft magnetic composite material of the present invention may be applied to various electronic devices, particularly devices having high frequency and microwave band operating frequencies. Accordingly, some embodiments of the present invention also provide an electronic device that includes a circuit and an insulated magnetic component disposed proximate to the circuit. For example, depending on the different electronic devices, the circuit may be a coil, a resonant circuit, etc., and the insulated magnetic component arranged next to the circuit may be a core, etc., which may be made of the soft magnetic composite material according to the above-described embodiment of the present invention, which may have a degree of planar orientation of 95% or more. Examples of such electronic devices include, but are not limited to, inductors, antennas, microwave isolators, microwave circulators, phase shifters, filters, and transformers, among others. Since the structures of these devices are known, the description will not be repeated here. In other embodiments of the present invention, electronic devices including these electronic devices are also provided.
The foregoing describes the general principles of the present application in conjunction with specific embodiments, however, it is noted that the advantages, effects, etc. mentioned in the present application are merely examples and are not limiting, and they should not be considered essential to the various embodiments of the present application. Furthermore, the foregoing disclosure of specific details is for the purpose of illustration and description and is not intended to be limiting, since the foregoing disclosure is not intended to be exhaustive or to limit the disclosure to the precise details disclosed.
The block diagrams of devices, apparatuses, systems referred to in this application are only given as illustrative examples and are not intended to require or imply that the connections, arrangements, configurations, etc. must be made in the manner shown in the block diagrams. These devices, apparatuses, devices, systems may be connected, arranged, configured in any manner, as will be appreciated by those skilled in the art. Words such as "including," "comprising," "having," and the like are open-ended words that mean "including, but not limited to," and are used interchangeably therewith. The words "or" and "as used herein mean, and are used interchangeably with, the word" and/or, "unless the context clearly dictates otherwise. The word "such as" is used herein to mean, and is used interchangeably with, the phrase "such as but not limited to".
It should also be noted that in the devices, apparatuses, and methods of the present application, the components or steps may be decomposed and/or recombined. These decompositions and/or recombinations are to be considered as equivalents of the present application.
The previous description of the disclosed aspects is provided to enable any person skilled in the art to make or use the present application. Various modifications to these aspects will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other aspects without departing from the scope of the application. Thus, the present application is not intended to be limited to the aspects shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
The foregoing description has been presented for purposes of illustration and description. Furthermore, the description is not intended to limit embodiments of the application to the form disclosed herein. While a number of example aspects and embodiments have been discussed above, those of skill in the art will recognize certain variations, modifications, alterations, additions and sub-combinations thereof.

Claims (14)

1. A method for preparing a soft magnetic composite material, comprising:
preparing easy-to-surface magnetic powder of a soft magnetic material, wherein the magnetic powder has an easy-to-magnetize surface;
preparing the easy-to-surface magnetic powder of the soft magnetic material and the binding material into mixed slurry according to a preset proportion;
orienting easy-to-magnetize surfaces of the easy-to-surface magnetic powder in the mixed slurry to be arranged in parallel along the external magnetic field; and
drying and hot-pressing the mixed slurry to prepare a soft magnetic composite material,
wherein, the easy-to-surface magnetic powder for preparing the soft magnetic material comprises:
preparing microparticles of a soft magnetic material;
heat-treating the microparticles of the soft magnetic material to relieve stress;
carrying out ball milling treatment on the microparticles of the soft magnetic material to prepare the easy-to-wear magnetic powder; and
washing, filtering and drying the easy-to-surface magnetic powder of the soft magnetic material; or,
the easy-to-surface magnetic powder for preparing the soft magnetic material comprises the following components:
depositing a sacrificial layer on a substrate;
depositing a soft magnetic material layer on the sacrificial layer;
etching the soft magnetic material layer to divide it into a plurality of regions having desired sizes;
removing the sacrificial layer to strip the soft magnetic material layer from the substrate to obtain easy-surface magnetic powder of the soft magnetic material; and
and washing, filtering and drying the easy-to-surface magnetic powder of the soft magnetic material.
2. The method of claim 1, wherein the soft magnetic material is Fe1-xNixAnd x is in the range of 0.35 to 0.9.
3. The method of claim 1, wherein the in-plane orientation of magnetic moments within the easy-to-surface magnetic powder of the soft magnetic material in the soft magnetic composite material is greater than 95%.
4. The method of claim 1, wherein the soft magnetic material has an easy-to-surface magnetic powder having a diameter-thickness ratio of 40 to 150.
5. The method of claim 1, wherein the bonding material comprises one or more of polyurethane, epoxy, polyimide.
6. The method of claim 1, wherein the easy-surface magnetic powder of the soft magnetic material accounts for 30% to 65% of a total volume of the easy-surface magnetic powder of the soft magnetic material and the binder material in the mixed slurry.
7. A method according to claim 1, wherein the microparticles of soft magnetic material have a particle size of 10-50 μm.
8. The method of claim 1, wherein the heat treatment temperature for heat-treating the microparticles of soft magnetic material is in the range of 250 ℃ to 500 ℃.
9. The method of claim 1, wherein the sacrificial layer comprises an aluminum layer and removing the sacrificial layer comprises etching the aluminum layer with an alkaline solution.
10. The method of claim 8, wherein the alkali solution comprises one or more of a sodium hydroxide solution and a potassium hydroxide solution.
11. The method according to claim 1, wherein the mixed slurry is subjected to a drying process while applying the external magnetic field to the mixed slurry to align the easy-to-magnetize planes of the easy-to-plane magnetic powder in parallel.
12. The method of claim 1, wherein the hot-pressing the dried mixed slurry comprises pressing in a direction perpendicular to the easy magnetization surface of the easy-to-surface magnetic powder.
13. A soft magnetic composite material prepared by the method of any one of claims 1 to 12.
14. An electronic device comprising an insulated magnetic component made of the soft magnetic composite material of claim 13.
CN202110981631.6A 2021-08-25 2021-08-25 Soft magnetic composite material and preparation method thereof Pending CN113643893A (en)

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Application publication date: 20211112