CN114496444A - Soft magnetic composite material and method for producing the same - Google Patents
Soft magnetic composite material and method for producing the same Download PDFInfo
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- CN114496444A CN114496444A CN202210215366.5A CN202210215366A CN114496444A CN 114496444 A CN114496444 A CN 114496444A CN 202210215366 A CN202210215366 A CN 202210215366A CN 114496444 A CN114496444 A CN 114496444A
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets 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
- H01F1/14—Magnets 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
- H01F1/147—Alloys characterised by their composition
-
- 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
- H01F41/02—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 for manufacturing cores, coils, or magnets
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The application provides a soft magnetic composite material, which comprises a core and a shell at least partially wrapping the core, wherein the material of the core comprises a first soft magnetic material, the material of the shell comprises a second soft magnetic material, the first soft magnetic material is an amorphous soft magnetic material or a nanocrystalline soft magnetic material, and the second soft magnetic material is a crystalline metal soft magnetic material. The soft magnetic composite material has the performance advantages of the core and the shell, so that the soft magnetic composite material has excellent magnetic performance and mechanical performance and is beneficial to application. The application also provides a method for preparing the soft magnetic composite material.
Description
Technical Field
The application belongs to the technical field of magnetic materials, and particularly relates to a soft magnetic composite material and a preparation method thereof.
Background
Soft magnetic materials are easily magnetized and demagnetized, and are widely used in devices for electronic equipment. At present, some soft magnetic materials have low resistivity and large eddy current loss, and some soft magnetic materials have low saturation induction strength and are not beneficial to the use of electronic equipment; some soft magnetic materials have too high hardness, which is not favorable for the molding and preparation of magnetic parts and affects the application of the magnetic parts in electronic equipment. Therefore, the development of soft magnetic materials having excellent magnetic properties and suitable mechanical properties has become a problem to be solved.
Disclosure of Invention
In view of this, the present application provides a soft magnetic composite material and a method for preparing the same.
In a first aspect, the present application provides a soft magnetic composite material, including a core and an outer shell at least partially wrapping the core, where a material of the core includes a first soft magnetic material, a material of the outer shell includes a second soft magnetic material, the first soft magnetic material is an amorphous soft magnetic material or a nanocrystalline soft magnetic material, and the second soft magnetic material is a crystalline soft magnetic metal material.
In a second aspect, the present application provides a method for preparing a soft magnetic composite material, comprising:
placing a core material and a target material into a container, wherein the cross section of an inner cavity of the container is polygonal, the core material comprises a first soft magnetic material, and the first soft magnetic material is an amorphous soft magnetic material or a nanocrystalline soft magnetic material;
rotating the container around a direction perpendicular to the section of the inner cavity, keeping the target material fixed, depositing the material of the target material on the surface of the core material through physical vapor deposition to form a shell at least partially wrapping the core material, so as to obtain the soft magnetic composite particles, wherein the material of the shell comprises a second soft magnetic material, and the second soft magnetic material is a crystalline metal soft magnetic material.
The application provides a soft magnetic composite material with a core-shell structure, wherein the material of a core comprises a first soft magnetic material, the material of a shell comprises a second soft magnetic material, and the microscopic morphologies of the first soft magnetic material and the second soft magnetic material are different, so that the properties of the core and the shell are different, and therefore the soft magnetic composite material has the performance advantages of both the core and the shell, has excellent magnetic property and mechanical property, and expands the application range of the soft magnetic composite material; the preparation method of the soft magnetic composite material is simple, convenient to operate and beneficial to use.
Drawings
In order to more clearly explain the technical solution in the embodiments of the present application, the drawings that are required to be used in the embodiments of the present application will be described below.
Fig. 1 is a schematic structural view of a soft magnetic composite material according to an embodiment of the present application.
Fig. 2 is a schematic structural view of a soft magnetic composite material according to another embodiment of the present application.
Fig. 3 is a schematic structural view of a soft magnetic composite material according to still another embodiment of the present application.
Fig. 4 is a schematic flow chart of a method for producing a soft magnetic composite according to an embodiment of the present disclosure.
Fig. 5 is a schematic cross-sectional view of a container provided in an embodiment of the present application.
Fig. 6 is a schematic view of a container according to an embodiment of the present disclosure during use.
Fig. 7 is a schematic flow chart of a method for producing a soft magnetic composite according to still another embodiment of the present application.
Description of reference numerals:
the magnetic core comprises a core 11, a shell 12, a first layer of shell 12 ', a second layer of shell 12', an insulating layer 13, a soft magnetic composite material 10, an inner cavity 21, a container 20, a core material 30 and a target material 40.
Detailed Description
The following is a preferred embodiment of the present application, and it should be noted that, for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present application, and these improvements and modifications are also considered as the protection scope of the present application.
The following disclosure provides many different embodiments or examples for implementing different features of the application. In order to simplify the disclosure of the present application, specific example components and arrangements are described below. Of course, they are merely examples and are not intended to limit the present application. Moreover, the present application may repeat reference numerals and/or letters in the various examples, such repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, examples of various specific processes and materials are provided herein, but one of ordinary skill in the art may recognize applications of other processes and/or use of other materials.
Referring to fig. 1, a schematic structural diagram of a soft magnetic composite material according to an embodiment of the present disclosure is shown, in which a soft magnetic composite material 10 includes a core 11 and a shell 12 at least partially wrapping the core 11, a material of the core 11 includes a first soft magnetic material, a material of the shell 12 includes a second soft magnetic material, the first soft magnetic material is an amorphous soft magnetic material or a nanocrystalline soft magnetic material, and the second soft magnetic material is a crystalline soft magnetic metal material.
It is understood that the soft magnetic material generally refers to a magnetic material having a coercive force (Hc) of not more than 1000A/m, and the micro morphology of the soft magnetic material has three states of crystalline, amorphous, and nanocrystalline. At present, the performance of soft magnetic materials still needs to be improved, for example, the resistivity of iron is low, the eddy current loss is large under an alternating magnetic field, and other elements are added to form an iron-based crystalline alloy, so that the resistivity is improved, the eddy current loss is reduced, and the saturation magnetization is also reduced; the amorphous soft magnetic material has low coercive force and low loss, the saturation magnetization and magnetic permeability of the nanocrystalline soft magnetic material are improved compared with those of the amorphous soft magnetic material, and the resistivity of the nanocrystalline soft magnetic material is equivalent to that of the amorphous soft magnetic material. The soft magnetic composite material 10 of the present application has a core-shell structure, and the inner core 11 has an amorphous soft magnetic material or a nanocrystalline soft magnetic material, that is, the microscopic morphology of the first soft magnetic material is an amorphous state or a nanocrystalline state, the atomic arrangement in the amorphous soft magnetic material has a short-range order and a long-range disorder state, and the nanocrystalline state contains crystal grains other than the crystalline state and the amorphous state. The amorphous soft magnetic material or the nanocrystalline soft magnetic material has low coercive force and low loss, and contributes to reducing the loss of the soft magnetic composite material 10; the shell 12 has a crystalline soft magnetic metal material, that is, the second soft magnetic material has a crystalline microscopic form, and atoms in the crystalline soft magnetic material are arranged in order, so that the crystalline soft magnetic metal material has high saturation magnetization and magnetic permeability and excellent plasticity, which is beneficial to improving the saturation magnetization and magnetic permeability of the soft magnetic composite material 10 and improving the plasticity of the soft magnetic composite material 10, and is beneficial to processing and forming the soft magnetic composite material 10, thereby improving the comprehensive magnetic property and comprehensive mechanical property of the soft magnetic composite material 10, and being beneficial to application of the soft magnetic composite material 10.
The crystalline soft magnetic material has high saturation magnetization and magnetic permeability, and the crystalline soft magnetic metal material has high saturation magnetization and magnetic permeability and good plasticity, thereby being beneficial to processing and molding of the soft magnetic composite material 10. In an embodiment of the present application, the crystalline metallic soft magnetic material includes at least one of iron, nickel, cobalt, iron-silicon alloy, iron-aluminum alloy, iron-nickel alloy, and iron-cobalt alloy. In one embodiment, the content of si in the fe-si alloy may be 0.5% to 4%, such as 1%, 2%, 3%, or 4%. In one embodiment, the aluminum content of the fe-al alloy may be 6% to 16%, such as 11.7%, 12%, 15%, 15.9%, or 16%. Further, the iron-aluminum alloy can also contain molybdenum; the content of molybdenum element can be 2% -3%, such as 2%, 2.4%, 2.8% or 3%. In one embodiment, the nickel content of the iron-nickel alloy may be 35% to 90%, such as 45%, 50%, 68%, or 78.5%. Furthermore, the iron-nickel alloy can also contain molybdenum; the content of molybdenum element is less than or equal to 5%, such as 2%, 3%, 4% or 5%. In one embodiment, the cobalt content in the iron-cobalt alloy may be 30% to 70%, such as 40%, 50%, 60%, or 65%. Furthermore, the iron-cobalt alloy can also contain vanadium; the content of vanadium element is less than or equal to 5%, such as 1%, 1.5%, 2% or 2.5%.
In the embodiments of the present application, the amorphous soft magnetic material includes at least one of an iron-based amorphous soft magnetic material, a cobalt-based amorphous soft magnetic material, and an iron-nickel-based amorphous soft magnetic material. In an embodiment, the Fe-based amorphous soft magnetic material may comprise at least one of a FeB amorphous material, a FeBC amorphous material, a FeSiB amorphous material, a fesibsi amorphous material, a FeCrSiB amorphous material, a FeCrSiBC amorphous material, and a fecosbsi, such as Fe80B20、Fe84B10C6、Fe86B7C7、Fe78Si13B9、Fe82Si10B8、Fe84Si10B6、Fe81Si3.5B13.5C2、Fe67Co18B14Si, etc. In one embodiment, the cobalt-based amorphous soft magnetic materialThe material may include at least one of a CoFeSiB amorphous material, a CoFeCrSiB amorphous material, a CoFeMoSiB amorphous material, a CoFeNiSiB amorphous material, and a CoFeNiNbSiB amorphous material, such as Co65.7Fe4.3Si17B13、Co70.3Fe4.7Si10B15、Co66Fe5Cr9Si5B15、Co66Fe4Mo2Si16B12、Co71.6Fe4.2Ni4.2Si10B10、Co66Fe4.5Ni2.3Nb2.2Si10B15And the like. In an embodiment, the iron-nickel based amorphous soft magnetic material may include at least one of a FeNiBP amorphous material, a FeNiMoB amorphous material, a FeNiSiB amorphous material, and a FeNiMoSiB amorphous material, such as Fe40Ni40B6P14、Fe40Ni38Mo4B18、Fe46.8Ni31.2Si10B12、Fe62.4Ni15.6Mo2Si8B12And the like.
In an embodiment of the present application, the nanocrystalline soft magnetic material comprises at least one of a FeZrB nanocrystalline material, a FeZrCuB nanocrystalline material, a FeHfB nanocrystalline material, a FeNbB nanocrystalline material, a FeNbZrCuB nanocrystalline material, a FeNbCuSiB nanocrystalline material, and a FeCuSiBP nanocrystalline material, such as Fe91Zr7B2、Fe90Zr7B3、Fe89Zr7CuB3、Fe86Zr7CuB6、Fe89Hf7B4、Fe84Nb7B9、Fe73.5Nb3CuSi13.5B9、Fe74Nb3CuSi16B6And the like. In the present application, the nanocrystalline soft magnetic material has nanocrystalline grains therein, and the grain size of the nanocrystalline grains may be, but not limited to, less than 15nm, such as 6nm to 8nm, 8nm to 10nm, or 10nm to 12nm, and the like.
In the present embodiment, the particle size of the core 11 is 2 μm to 50 μm, ensuring the performance of the soft magnetic composite material 10 and facilitating the coating of the shell 12. Specifically, the particle size of the core 11 may be, but not limited to, 2 μm, 8 μm, 15 μm, 20 μm, 25 μm, 32 μm, 37 μm, 40 μm, 45 μm, or 50 μm. In one embodiment, the particle size of the inner core 11 is 2 μm to 10 μm. In another embodiment, the particle size of the inner core 11 is 20 μm to 30 μm. In yet another embodiment, the particle size of the inner core 11 is 40 μm to 50 μm.
In the present embodiment, the thickness of the outer shell 12 is 5nm to 1000 nm. Specifically, the thickness of the housing 12 may be, but is not limited to, 5nm, 50nm, 180nm, 300nm, 500nm, 750nm, 830nm, 950nm, 1000nm, or the like. In one embodiment, the thickness of the housing 12 is 5nm to 100 nm. In another embodiment, the thickness of the housing 12 is 300nm-500 nm. In yet another embodiment, the thickness of the housing 12 is 800nm to 1000 nm. It is understood that the soft magnetic composite material 10 may include a single layer of the outer shell 12, or may include multiple layers of the outer shell 12 (e.g., two, three, four, five, six, etc.), and the materials of the multiple layers of the outer shell 12 may be the same or different. Referring to fig. 2, a schematic structural diagram of a soft magnetic composite material 10 according to another embodiment of the present disclosure is shown, in which the soft magnetic composite material 10 includes a core 11 and two shells 12 wrapping the core 11, the two shells 12 are respectively a first shell 12 ' and a second shell 12 ", the first shell 12 ' wraps the core 11, and the second shell 12" wraps the first shell 12 '. While fig. 2 shows the soft magnetic composite material 10 having a two-layered outer shell 12, it is to be understood that the soft magnetic composite material 10 may also have three or more layers of outer shell 12, which will not be described in detail herein. In one embodiment, soft magnetic composite 10 includes multiple layers of shells 12, with adjacent shells 12 being of different materials, thereby further improving the magnetic and mechanical properties of soft magnetic composite 10. In the present application, the outer shell 12 may completely cover the inner core 11, i.e. the coverage rate is 100%; the shell 12 may also cover a portion of the core 11, such as a coverage rate greater than 80%, greater than 90%, greater than 95%, greater than 98%, greater than 99%, etc.
The amorphous/nanocrystalline soft magnetic material has high hardness and low plasticity, and when the amorphous/nanocrystalline soft magnetic material is used for preparing a magnetic part, substances such as resin and the like are required to be added for forming so as to prevent the amorphous/nanocrystalline soft magnetic material from cracking in the pressing process to influence the magnetic property of the amorphous/nanocrystalline soft magnetic material, however, the addition of the substances such as resin and the like reduces the magnetic property of the magnetic part. According to the application, the eddy current loss of the soft magnetic composite material 10 can be reduced by adopting the amorphous/nanocrystalline soft magnetic material, the high magnetic induction strength and the magnetic permeability of the soft magnetic composite material 10 can be ensured by adopting the crystalline metal soft magnetic material, meanwhile, the crystalline metal soft magnetic material is wrapped, the plasticity of the soft magnetic composite material 10 is improved, the pressing of the soft magnetic composite material 10 is facilitated, the pressing difficulty is reduced, the processing and forming operation of the soft magnetic composite material 10 is facilitated, no other non-magnetic substance is added, the content of the soft magnetic material in the soft magnetic composite material 10 is ensured, and the magnetic performance of the soft magnetic composite material is improved. In an embodiment of the present application, the first soft magnetic material is an amorphous soft magnetic material, and the second soft magnetic material is a crystalline metallic soft magnetic material. In another embodiment of the present application, the first soft magnetic material is a nanocrystalline soft magnetic material and the second soft magnetic material is a crystalline metallic soft magnetic material. In one embodiment, the crystalline metallic soft magnetic material comprises at least one of iron, an iron-nickel alloy, and an iron-cobalt alloy. The crystalline metal soft magnetic material has high magnetic induction strength and magnetic permeability, is excellent in plasticity, and is beneficial to subsequent compression molding operation. In one embodiment, the crystalline metallic soft magnetic material is an iron-nickel alloy. The selection of an iron-nickel alloy enables the housing 12 to have high plasticity, which facilitates subsequent press forming operations.
In the embodiments of the present application, the hardness of the first soft magnetic material is greater than that of the second soft magnetic material, and the plasticity of the second soft magnetic material is greater than that of the first soft magnetic material. Wherein the plasticity can be characterized by the elongation. The soft magnetic composite material 10 formed by using soft magnetic materials having different mechanical properties is advantageous for the compression of the soft magnetic composite material 10, thereby facilitating the production of a magnetic article.
Referring to fig. 3, a schematic structural diagram of a soft magnetic composite material 10 according to another embodiment of the present application is substantially the same as that shown in fig. 1, except that the soft magnetic composite material 10 further includes an insulating layer 13, and the insulating layer 13 at least partially wraps the outer shell 12. By providing the insulating layer 13, the electrical resistivity of the soft magnetic composite material 10 is increased, and the eddy current loss of the soft magnetic composite material 10 in a magnetic field is reduced, which is advantageous for use in a high-frequency environment. In the present application, the insulating layer 13 may completely cover the housing 12, i.e. the coverage rate is 100%; the insulating layer 13 may also cover a portion of the housing 12, such as a coverage rate greater than 80%, greater than 90%, greater than 95%, greater than 98%, greater than 99%, etc. In one embodiment, the insulating layer 13 completely covers the outer shell 12, minimizing eddy current losses in the soft magnetic composite 10.
In the present embodiment, the material of the insulating layer 13 includes at least one of a ceramic material and ferrite. The insulating layer 13 has high temperature resistance, high toughness, and high resistivity, and can not only play an insulating role, reduce the eddy current loss of the soft magnetic composite material 10, but also facilitate the subsequent press molding operation. When the organic insulating layer is formed by a coating resin or the like, the content of the soft magnetic material in the soft magnetic composite material 10 is reduced, resulting in a decrease in magnetic permeability and an increase in hysteresis loss, and affecting the temperature of press molding; when other inorganic metal or nonmetal materials are used for forming the insulating layer, the surface hardness of the soft magnetic composite material can be increased, and the insulating layer can even crack in the forming process of the magnetic part, so that the forming difficulty is further increased. In one embodiment, the ceramic material comprises at least one of zirconia, yttria, alumina, and silicon carbide. The ceramic material has high resistivity, excellent insulating property and toughness, and is beneficial to improving the performance of the soft magnetic composite material 10. In one embodiment, the insulating layer 13 is made of zirconia and yttria, wherein the yttria stabilizes the zirconia, so that the insulating layer 13 has excellent insulating property and high temperature resistance. Ferrite, which is a soft magnetic material having iron oxide as a main component and formed by compounding with other metal oxides such as ZnO, NiO, MnO and the like, is a metal oxide material of ceramic type, and has a high specific resistance, especially when 2-valent metal oxides such as manganese, nickel, cobalt, zinc and the like are contained in ferrite, the ferrite can have a high specific resistance (e.g., 10%4Ω · cm, etc.). Specifically, the ferrite may include ferromanganeseAt least one of ferrite, zinc ferrite, manganese magnesium zinc ferrite, nickel zinc ferrite, and copper zinc ferrite. For example, nickel zinc ferrite has a saturation magnetization of 0.2T to 0.8T. In one embodiment, the insulating layer 13 is made of ferrite. By using ferrite as the insulating layer 13, the content of the soft magnetic material in the soft magnetic composite material 10 is increased, and the ferrite is resistant to high temperature, contributes to increasing the molding temperature, contributes to reducing the residual stress during press molding, and reduces the coercive force, and is advantageous for use of the soft magnetic composite material 10.
In the embodiment of the present application, the thickness of the insulating layer 13 is 5nm to 100nm, which is beneficial to increase the resistivity of the soft magnetic composite material 10, thereby reducing the eddy current loss thereof, improving the high temperature resistance thereof, and ensuring the service performance thereof. Specifically, the thickness of the insulating layer 13 may be, but not limited to, 5nm, 10nm, 20nm, 33nm, 40nm, 45nm, 55nm, 70nm, 80nm, 95nm, 100nm, or the like. In one embodiment, the thickness of the insulating layer 13 is 5nm to 20 nm. In another embodiment, the thickness of the insulating layer 13 is 30nm-60 nm. In yet another embodiment, the thickness of the insulating layer 13 is 80nm-100 nm.
In the present embodiment, the soft magnetic composite 10 further includes a binder that wraps the outer shell 12 or the insulating layer 13. The addition of the binder facilitates the fixation of the soft magnetic composite material 10 and facilitates the processing and molding. In one embodiment, the mass content of the binder in the soft magnetic composite material 10 is 1% to 10%, such as 1% to 7%, 1% to 5%, or 2% to 3%, etc., of the mass content of the binder in the soft magnetic composite material 10, thereby facilitating the compression molding of the soft magnetic composite material 10 without reducing the density of the soft magnetic material in the soft magnetic composite material 10. In the present application, a substance having viscosity may be selected as the binder. In one embodiment, the binder may be a resin, such as at least one of polyimide resin, epoxy resin, silicone resin, and fluorine resin. In a particular embodiment, the binder may be a thermosetting resin.
The present application also provides a method for producing a soft magnetic composite material for use in producing the soft magnetic composite material 10 of any of the above embodiments. Referring to fig. 4, a schematic flow chart of a method for preparing a soft magnetic composite according to an embodiment of the present application includes:
s101: the core material and the target material are placed in a container, the cross section of an inner cavity of the container is polygonal, the core material comprises a first soft magnetic material, and the first soft magnetic material is an amorphous soft magnetic material or a nanocrystalline soft magnetic material.
S102: and rotating the container around the direction vertical to the section of the inner cavity, keeping the target material fixed, depositing the material of the target material on the surface of the core material through physical vapor deposition to form a shell at least partially wrapping the core material so as to obtain the soft magnetic composite particles, wherein the material of the shell comprises a second soft magnetic material, and the second soft magnetic material is a crystalline metal soft magnetic material.
In S101, please refer to fig. 5, which is a schematic cross-sectional view of a container 20 according to an embodiment of the present disclosure, the container 20 has an inner cavity 21, and the cross-section of the inner cavity 21 is a polygon. Referring to fig. 6, a schematic illustration of a container 20 according to an embodiment of the present disclosure is shown in use, wherein a core material 30 and a target 40 are disposed in the container 20 so as to form a shell 12 on a surface of the core material 30. It is understood that the core material 30 is the core 11 of the soft magnetic composite material 10, and the selection of the material, the micro-morphology, the particle size, etc. is not described herein again. In one embodiment, the cross-section of the cavity 21 of the container 20 is parallel to the direction of gravity. In another embodiment, the cross-section of the cavity 21 of the container 20 is perpendicular to the direction of gravity. In the present embodiment, a target holder is disposed in the inner cavity 21 of the container 20, and the target holder is used for placing the target 40. In the present application, the inner cavity 21 of the container 20 is a vacuum chamber for facilitating deposition of the target 40, and the selection of the target 40 is determined according to the material of the housing 12. In the embodiment of the present application, when the housing 12 is made of an alloy material, the target material 40 may be an alloy target, or may be a plurality of elemental metal targets.
In the present application, the core material 30 may be prepared or may be purchased directly. In one embodiment, the amorphous soft magnetic material may be prepared by a magnetic film pulverization method or a water mist spray method, and the prepared amorphous soft magnetic material may be used as the first soft magnetic material. The magnetic film pulverizing method is to pulverize and grind an amorphous alloy magnetic film with a micron-sized thickness (several tens of microns, etc.) into a metal powder state, thereby obtaining an amorphous soft magnetic material. The water mist spraying method is to spray and atomize liquid metal in a high-temperature molten state and high-pressure water or air at the same time, and the high-temperature liquid metal is quenched to form amorphous fine particles so as to obtain the amorphous soft magnetic material. The water mist spraying method can obtain the amorphous soft magnetic material with good sphericity, which is more beneficial to the deposition and coating of the target material 40. In one embodiment, the amorphous soft magnetic material is prepared by a water mist spraying method, and the particle size of the amorphous soft magnetic material is 2 μm to 50 μm. In one embodiment, a small amount of Zr, Cu, Hf, Nb, or other elements may be added to the amorphous soft magnetic material, and crystallization may be performed at an appropriate temperature to precipitate a partial nano-scale crystal phase, thereby obtaining a nano-crystalline soft magnetic material.
In S102, the container 20 rotates around a direction perpendicular to the cross section of the cavity 21, and in the rotating process, the core material 30 in the cavity 21 is continuously turned over under the action of gravity, so that the target material 40 is deposited on the surface of the core material 30 by setting the material of the target material 40 to perform physical vapor deposition, and finally the required shell 12 is formed; in the deposition process, the core material 30 is moved all the time under the action of the rotating inner cavity 21 and gravity, so that the target material 40 can be uniformly deposited on the surface of the core material 30 to form the shell 12 uniformly coating the core material 30. It will be appreciated that by changing the material of the target 40, a multi-layered shell 12 of different material composition can be obtained, and by controlling the deposition time, a shell 12 of the desired thickness can be obtained. The target material 40 is fixed, and the movement range of the core material 30 in the inner cavity 21 and the deposition range of the target material 40 have an overlapped area, so that the formation of the shell 12 is ensured. The container 20 may be rotated about its center axis as a rotation axis, and as shown in fig. 6, the container 20 may be rotated counterclockwise, may be rotated clockwise, or may be rotated clockwise and counterclockwise alternately. In the embodiment of the present application, the rotation speed of the container 20 is 20rpm to 40rpm, so as to ensure that the core material 30 will move during the rotation of the container 20, and the displacement will not be too large, which is beneficial to the deposition of the target material 40. Specifically, the rotation speed of the vessel 20 is 20rpm, 25rpm, 30rpm, 35rpm, 40rpm, or the like.
In the present application, the physical vapor deposition can be, but is not limited to, vacuum evaporation, vacuum sputtering, ion plating, etc., and the process conditions of the physical vapor deposition can be selected according to the properties of the deposited target 40. In this way, the core material 30 and the target material 40 can be selected as needed, and the soft magnetic composite material 10 having excellent overall performance can be obtained. In the present embodiment, the target 40 is disposed, and gas is introduced to adjust the output power and the pressure of the inner cavity 21 for physical vapor deposition. Specifically, the output power may be 100W-300W, such as 100W, 160W, 200W, 250W, 270W, or 300W; the pressure of the inner cavity 21 may be 0.1Pa to 5Pa, such as 0.1Pa, 0.5Pa, 1Pa, 1.5Pa, 2Pa, 3Pa, 4Pa, 5Pa, etc.; when the material of the housing 12 does not contain oxygen or carbon, the introduced gas is inert gas; when the material of the housing 12 contains oxygen, a mixed gas is introduced, where the mixed gas includes an inert gas and oxygen, the content of oxygen in the mixed gas may be 20% to 50%, such as 20%, 25%, 30%, 35%, 40%, 45%, or 50%, and the inert gas may be, but is not limited to, argon, helium, nitrogen, and the like. In the embodiment of the present invention, the core material 30 is heated during the physical vapor deposition process to make the temperature of the core material 30 be 100-400 ℃ (e.g., 100 ℃, 150 ℃, 200 ℃, 250 ℃, 300 ℃, 350 ℃, or 400 ℃), which is beneficial to the deposition of the target material 40 and improves the bonding force between the core 11 and the shell 12. In the embodiment of the present application, the core material 30 and the target 40 are placed in the container 20, and the target 40 is an iron-nickel alloy, wherein the content of nickel element in the iron-nickel alloy may be 50% to 80%; introducing inert gas, adjusting the pressure of the inner cavity 21 to be 0.1-5.0 Pa, and carrying out physical vapor deposition under the conditions that the output power is 100-300W and the rotating speed of the container 20 is 20-40 rpm to obtain soft magnetic composite particles, namely the soft magnetic composite material 10, wherein the shell 12 of the soft magnetic composite material 10 is made of iron-nickel alloy.
In one embodiment, the core material 30 and the target 40 are placed in the container 20, the cross section of the inner cavity 21 of the container 20 is polygonal, the core material 30 is an iron-based amorphous soft magnetic material, and the target 40 is an iron-nickel alloyGold, wherein the content of nickel element in the iron-nickel alloy can be 50% -80%; the interior 21 of the container 20 is vented to an internal pressure of 8 x 10-4Introducing argon gas to adjust the internal pressure to 0.1Pa-5.0Pa after Pa, performing sputtering at an output of 100W-300W, and rotating the container 20 at a rotation speed of 20rpm-40 rpm; after sputtering is finished, introducing nitrogen into the inner cavity 21 to atmospheric pressure, and taking out the soft magnetic composite material 10; the core 11 of the soft magnetic composite material 10 is made of an iron-based amorphous soft magnetic material, and the shell 12 is made of an iron-nickel alloy layer. The saturation magnetization of the Fe-based amorphous soft magnetic material is 1.2T-1.4T, and the maximum magnetic permeability is about 6 x 104The saturation magnetization of Fe-Ni alloy is 0.7T-0.8T, and the maximum magnetic permeability is about 3X 104The saturation magnetization of the soft magnetic composite material 10 is 1T-1.4T, and the maximum magnetic permeability is 3X 104The above. The soft magnetic composite material 10 obtained by the method provided by the application has excellent comprehensive magnetic performance, and the iron-nickel alloy improves the plasticity of the soft magnetic composite material 10, thereby being beneficial to the improvement and preparation of the magnetism of a magnetic part.
Referring to fig. 7, a schematic flow chart of a method for preparing a soft magnetic composite according to another embodiment of the present application includes:
s201: the core material and the target material are placed in a container, the cross section of an inner cavity of the container is polygonal, the core material comprises a first soft magnetic material, and the first soft magnetic material is an amorphous soft magnetic material or a nanocrystalline soft magnetic material.
S202: and rotating the container around the direction vertical to the section of the inner cavity, keeping the target material fixed, and depositing the material of the target material on the surface of the core material through physical vapor deposition to form a shell at least partially wrapping the core material, wherein the material of the shell comprises a second soft magnetic material, and the second soft magnetic material is a crystalline metal soft magnetic material.
S203: and forming an insulating layer on the surface of the shell, wherein the insulating layer at least partially wraps the shell to obtain the soft magnetic composite particles.
Please refer to the above descriptions of S101 and S102 for S201 and S202.
In S203, an insulating layer 13 may be formed on the surface of the case 12. In the present application, the insulating layer 13 is formed by a physical vapor deposition method. Specifically, the target 40 of a desired material is provided, and the desired insulating layer 13 is obtained. By the method, the selection range of the material of the insulating layer 13 can be widened, the material for improving the performance of the soft magnetic composite material 10 can be selected, and the controllability of the whole process and the structure of the soft magnetic composite material 10 is high.
In the embodiment of the present application, the material of the insulating layer includes at least one of a ceramic material and ferrite. In the present embodiment, the core material 30 with the outer shell 12 and the target 40 are placed in the container 20; introducing gas, adjusting the pressure of the inner cavity 21 to 0.1Pa-5.0Pa (such as 0.1Pa, 0.5Pa, 1Pa, 1.5Pa, 2Pa, 3Pa, 4Pa or 5 Pa), performing physical vapor deposition at an output power of 1000W-4000W (such as 1000W, 1500W, 2000W, 3000W, 3600W or 4000W) and a rotation speed of the container 20 of 20rpm-40rpm, and depositing an insulating layer 13 on the surface of the shell 12 to obtain the soft magnetic composite material 10, wherein the insulating layer 13 is made of a ceramic material. In one embodiment, a target 40 containing zirconium element and yttrium element is used, a mixed gas containing inert gas and oxygen is introduced into the inner cavity 21 of the container 20, the pressure of the inner cavity 21 is 0.1Pa-5.0Pa, the insulating layer 13 is deposited on the surface of the outer shell 12, and the material of the insulating layer 13 comprises zirconium oxide and yttrium oxide. Optionally, the mixed gas includes inert gas and oxygen, and the content of oxygen in the mixed gas is 20% to 50%, such as 20%, 25%, 30%, 35%, 40%, 45%, or 50%. The number of the targets 40 may be single or multiple, for example, the targets 40 include a zirconium target and a yttrium target. In one embodiment, the target 40 is an alloy comprising zirconium and yttrium, and the interior chamber 21 of the container 20 is evacuated to an internal pressure of 8 x 10-4Introducing a mixed gas of argon and oxygen after Pa is less than Pa, adjusting the oxygen content in the mixed gas to be 20% -50%, adjusting the internal pressure to be 0.1Pa-5.0Pa, sputtering under the output power of 1000W-4000W, starting rotating the container 20 at the rotating speed of 20rpm-40rpm, and forming an insulating layer 13 on the surface of the shell 12; after sputtering is finished, introducing nitrogen into the inner cavity 21 to atmospheric pressure, and taking out the soft magnetic composite material 10; the soft magnetic composite material 10 has an insulating layer 13. It is composed ofThe molar ratio of zirconium to yttrium in the target 40 may be, but is not limited to, 4.
In the present embodiment, a core material 30 having an outer shell 12 and a target material 40 are placed in a container 20, wherein the target material 40 is a ferrous alloy target; introducing mixed gas, adjusting the pressure of the inner cavity 21 to be 0.1-5.0 Pa (such as 0.1Pa, 0.5Pa, 1Pa, 1.5Pa, 2Pa, 3Pa, 4Pa or 5Pa, and the like), carrying out physical vapor deposition at an output power of 100-300W (such as 100W, 160W, 200W, 250W, 270W, 300W, and the like) and a rotation speed of the container 20 of 20-40 rpm, and depositing the insulating layer 13 on the surface of the shell 12 to obtain the soft magnetic composite material 10, wherein the insulating layer 13 is made of ferrite, the mixed gas comprises inert gas and oxygen, and the content of the oxygen in the mixed gas is 20-50% (such as 20%, 25%, 30%, 35%, 40%, 45%, 50%, and the like). In one embodiment, an iron-nickel-zinc alloy is used as the target 40, a mixed gas containing an inert gas and oxygen is introduced into the inner cavity 21 of the container 20, the pressure of the inner cavity 21 is 0.1Pa-5.0Pa, the insulating layer 13 is deposited on the surface of the outer shell 12, and the material of the insulating layer 13 includes nickel-zinc ferrite. In a specific embodiment, the core material 30 and the target material 40 are placed in the container 20, the cross section of the inner cavity 21 of the container 20 is polygonal, the core material 30 is an amorphous soft magnetic material, and the target material 40 is an iron-nickel alloy, wherein the content of nickel element in the iron-nickel alloy can be 50% -80%; the interior 21 of the container 20 is vented to an internal pressure of 8 x 10-4Introducing argon gas to adjust the internal pressure to 0.1Pa-5.0Pa after Pa, performing sputtering at an output of 100W-300W, and rotating the container 20 at a rotation speed of 20rpm-40 rpm; the target 40 is then replaced by Fe63Ni13Zn24Introducing mixed gas of argon and oxygen into an inner cavity 21 of the container 20, wherein the content of the oxygen in the mixed gas is 20-50%, adjusting the internal pressure to be 0.1-5.0 Pa, sputtering under the output power of 100-300W, and simultaneously starting to rotate the container 20 at the rotating speed of 20-40 rpm; after sputtering is finished, introducing nitrogen into the inner cavity 21 to atmospheric pressure, and taking out the soft magnetic composite material 10; the core 11 of the soft magnetic composite material 10 is made of amorphous soft magnetic material, the shell 12 is made of iron-nickel alloy shell, and the insulating layer 13 is made of nickel-zinc ferrite.
In the present embodiment, the method of producing the soft magnetic composite material 10 further includes dispersing the soft magnetic composite particles in a binder and performing press molding. Further, the mass content of the binder in the soft magnetic composite material 10 is 1% to 10%, which is advantageous for the compression molding of the soft magnetic composite material 10, and does not decrease the density of the soft magnetic composite particles in the soft magnetic composite material 10. It will be appreciated that without the press forming operation, the soft magnetic composite particles are the soft magnetic composite material 10. Specifically, the pressing may be performed in a mold, but not limited thereto. Soft magnetic composite particles with a shell 12 wrapping a core 11 or with an insulating layer 13 wrapping a shell 12 and a core 11 are obtained by physical vapor deposition, and a plurality of soft magnetic composite particles are mixed with a binder and then subjected to compression molding to obtain a soft magnetic composite material 10 with a certain shape, which can be used in electronic devices, such as a part of inductors, filters and transformers. Due to the wrapping of the shell 12 and/or the insulating layer 13, the soft magnetic composite particles have excellent mechanical properties, the structure of the soft magnetic composite particles cannot be damaged by external force in the compression molding process, the molding difficulty of the soft magnetic composite material 10 is reduced, the soft magnetic composite material 10 can be molded at one time, the operation is simple and convenient, and the soft magnetic composite material 10 in different shapes, such as E-shaped, U-shaped, L-shaped, annular and the like, can be obtained.
The preparation method of the soft magnetic composite material 10 is simple, easy to operate, high in process controllability, green and environment-friendly in preparation process, capable of expanding the selection range of the materials of the inner core 11 and the shell 12, more suitable for large-scale production of the soft magnetic composite material 10, high in product yield, excellent in magnetic performance and more beneficial to application of the soft magnetic composite material.
The foregoing detailed description has provided embodiments of the present application and is presented to enable the principles and embodiments of the present application to be illustrated and described, where the above description is merely intended to facilitate the understanding of the present application's methods and their core concepts; meanwhile, for a person skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.
Claims (13)
1. A soft magnetic composite material, comprising a core and a shell at least partially wrapping the core, wherein the core comprises a first soft magnetic material, the shell comprises a second soft magnetic material, the first soft magnetic material is an amorphous soft magnetic material or a nanocrystalline soft magnetic material, and the second soft magnetic material is a crystalline soft magnetic metal material.
2. A soft magnetic composite according to claim 1, wherein the amorphous soft magnetic material comprises at least one of an iron-based amorphous soft magnetic material comprising at least one of a FeB amorphous material, a FeBC amorphous material, a FeSiB amorphous material, a FeSiBC amorphous material, a fensbc amorphous material, a fenbbib amorphous material, a FeCrSiB amorphous material, a FeCrSiBC amorphous material, and a FeCoB, and wherein the cobalt-based amorphous soft magnetic material comprises at least one of a CoFeSiB amorphous material, a CoFeCrSiB amorphous material, a CoFeMoSiB amorphous material, a cofeniib amorphous material, and a cofenibsib amorphous material, and wherein the iron-nickel-based amorphous soft magnetic material comprises at least one of a febnp amorphous material, a femtob amorphous material, a feniib amorphous material, and a FeNiMoSiB amorphous material;
the nanocrystalline soft magnetic material comprises at least one of a FeZrB nanocrystalline material, a FeZrCuB nanocrystalline material, a FeHfB nanocrystalline material, a FeNbB nanocrystalline material, a FeNbZrCuB nanocrystalline material, a FeNbCuSiB nanocrystalline material and a FeCuSiBP nanocrystalline material;
the crystalline metallic soft magnetic material comprises at least one of iron, nickel, cobalt, iron-silicon alloy, iron-aluminum alloy, iron-nickel alloy and iron-cobalt alloy.
3. A soft magnetic composite as claimed in claim 1, characterized in that the particle size of the core is 2 μm to 50 μm and the thickness of the outer shell is 5nm to 1000 nm.
4. A soft magnetic composite as claimed in claim 1, comprising a plurality of the shells, adjacent to each other being of a different material.
5. A soft magnetic composite as claimed in any one of claims 1 to 4, further comprising an insulating layer at least partially surrounding the outer shell; the thickness of the insulating layer is 5nm-100 nm.
6. A soft magnetic composite as claimed in claim 5, wherein the insulating layer is made of a material including at least one of a ceramic material and ferrite;
wherein the ceramic material comprises at least one of zirconia, yttria, alumina, and silicon carbide; the ferrite comprises at least one of manganese ferrite, zinc ferrite, manganese-magnesium-zinc ferrite, nickel-zinc ferrite and copper-zinc ferrite.
7. A method for preparing a soft magnetic composite material, comprising:
placing a core material and a target material into a container, wherein the cross section of an inner cavity of the container is polygonal, the core material comprises a first soft magnetic material, and the first soft magnetic material is an amorphous soft magnetic material or a nanocrystalline soft magnetic material;
rotating the container around a direction perpendicular to the section of the inner cavity, keeping the target material fixed, depositing the material of the target material on the surface of the core material through physical vapor deposition to form a shell at least partially wrapping the core material, so as to obtain the soft magnetic composite particles, wherein the material of the shell comprises a second soft magnetic material, and the second soft magnetic material is a crystalline metal soft magnetic material.
8. The method of claim 7, wherein the container is rotated at a speed of 20rpm to 40 rpm;
heating the core material in the physical vapor deposition process to ensure that the temperature of the core material is 100-400 ℃.
9. The method of claim 7, further comprising forming an insulating layer on a surface of the housing, the insulating layer at least partially surrounding the housing; the material of the insulating layer comprises at least one of ceramic material and ferrite.
10. The method according to claim 9, wherein the target material containing zirconium element and yttrium element is used, a mixed gas containing an inert gas and oxygen is introduced into an inner cavity of the container, the pressure of the inner cavity is 0.1Pa to 5.0Pa, and the insulating layer is deposited on the surface of the outer shell, and the material of the insulating layer comprises zirconium oxide and yttrium oxide.
11. The preparation method according to claim 9, wherein an iron-nickel-zinc alloy is used as the target material, a mixed gas containing an inert gas and oxygen is introduced into an inner cavity of the container, the pressure of the inner cavity is 0.1Pa-5.0Pa, the insulating layer is deposited on the surface of the shell, and the material of the insulating layer comprises nickel-zinc ferrite.
12. The production method according to claim 7, wherein the amorphous soft magnetic material is produced by a water mist jet method, and the particle diameter of the amorphous soft magnetic material is 2 μm to 50 μm;
the target material is an iron-nickel alloy, and the content of nickel element in the iron-nickel alloy is 50% -80%.
13. The method according to claim 7, further comprising dispersing the soft magnetic composite particles in a binder and performing compression molding, wherein the binder is contained in the soft magnetic composite material in an amount of 1% to 10% by mass.
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| WO2024146572A1 (en) * | 2023-01-04 | 2024-07-11 | 雅安百图高新材料股份有限公司 | Composite material and preparation method therefor |
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