CN111863372B - Anti-electromagnetic interference soft magnetic particle film and preparation method thereof - Google Patents

Anti-electromagnetic interference soft magnetic particle film and preparation method thereof Download PDF

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CN111863372B
CN111863372B CN202010735170.XA CN202010735170A CN111863372B CN 111863372 B CN111863372 B CN 111863372B CN 202010735170 A CN202010735170 A CN 202010735170A CN 111863372 B CN111863372 B CN 111863372B
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soft magnetic
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magnetic film
sputtering
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CN111863372A (en
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邓毕力
潘振海
王玉川
徐敏义
罗顶飞
晋立从
张朋
王波
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Anhui Zhimagnetic New Material Technology Co Ltd
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    • 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
    • H01F1/33—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 mixtures of metallic and non-metallic particles; metallic particles having oxide skin
    • C—CHEMISTRY; METALLURGY
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3464—Sputtering using more than one target
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C24/00—Coating starting from inorganic powder
    • C23C24/02—Coating starting from inorganic powder by application of pressure only
    • C23C24/04—Impact or kinetic deposition of particles
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
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    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
    • C23C28/42—Coatings including alternating layers following a pattern, a periodic or defined repetition characterized by the composition of the alternating layers
    • 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
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • H05K9/0088—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising a plurality of shielding layers; combining different shielding material structure

Abstract

The invention provides an anti-electromagnetic interference soft magnetic particle film and a preparation method thereof, wherein the soft magnetic particle film is of a multilayer structure and comprises a middle two-phase nano-crystalline soft magnetic film and a plurality of overlapped repeating structures positioned at two sides of the two-phase nano-crystalline soft magnetic film, and each overlapped repeating structure comprises a nano ZnO layer and a nano hexagonal boron nitride layer; the structural formula of the biphase nanocrystalline soft magnetic film is ((Fe)zA1‑z)aCobQcBad)1‑x‑(RO2)x(ii) a The biphase nanocrystalline soft magnetic film is alpha- (Fe) with bbc structurezA1‑z)aCobQcBadNano metal particle is coated by RO2And the insulating medium nano-particle is wrapped in the structure. The invention adds RO2Alpha- (Fe) doped with bbc-wrapped structurezA1‑z)aCobQcBadThe nano metal effectively reduces the coercive force, improves the soft magnetic performance and is beneficial to the grain refinement of the film.

Description

Anti-electromagnetic interference soft magnetic particle film and preparation method thereof
Technical Field
The invention belongs to the technical field of electromagnetic materials, and particularly relates to an anti-electromagnetic interference soft magnetic particle film and a preparation method thereof.
Background
With the development of scientific technology, communication technologies such as mobile phones and high-speed wireless local area networks have realized real-time communication between people and any people anywhere, and meanwhile, the data transmission rate of wireless communication technologies reaches the frequency band. For example, bluetooth is operating in the frequency band. Wireless mobile devices are rapidly moving towards more miniaturization and miniaturization in order to achieve higher and faster mobility of wireless systems. The rf circuit, which consists of two boards, a transmission circuit and a reception circuit, is a core component of a wireless system, and is favored in signal amplifiers, filters and modems due to its high integration. The widespread use of radio frequency circuits in mobile devices requires a large number of passive components, mainly capacitors and inductors. With the demand for miniaturization and high performance of devices, there is an increasing demand for soft magnetic thin films having high magnetic permeability, high saturation magnetization, low coercive force, and high resistivity.
The results of the study show that in order to maintain excellent high-frequency characteristics, the magnetic material is required to have a large resistivity ρ and a large saturation magnetization Ms and also to have an anisotropy field Hk of a moderate magnitude. On the other hand, high-density and wide-spectrum electromagnetic signals generated by the conventional integrated electronic device in operation fill the whole space to form a complex electromagnetic environment, so that the electronic equipment and the power supply are required to have good electromagnetic compatibility in each frequency band and in a use temperature range, and a series of challenges are brought to the anti-electromagnetic interference technology.
Disclosure of Invention
Aiming at the defects, the invention provides the anti-electromagnetic interference soft magnetic particle film which has good magnetic conductivity and high resistivity at high temperature, can be suitable for a high-frequency band and has a properly large uniaxial anisotropic field, and the preparation method thereof.
The invention provides the following technical scheme: the anti-electromagnetic interference soft magnetic particle film is characterized in that the soft magnetic particle film is of a multilayer structure and comprises a middle two-phase nano-crystalline soft magnetic film, a plurality of overlapped repeating structures positioned on the upper side of the two-phase nano-crystalline soft magnetic film and a plurality of overlapped repeating structures positioned on the lower side of the two-phase nano-crystalline soft magnetic film, wherein one overlapped repeating structure comprises a nano ZnO layer and a nano hexagonal boron nitride layer;
the structural formula of the biphase nanocrystalline soft magnetic film is ((Fe)zA1-z)aCobQcBad)1-x-(RO2)xWherein a is more than or equal to 30 and less than or equal to 60, b is more than or equal to 50 and less than or equal to 70, c is more than or equal to 10 and less than or equal to 30, d is more than or equal to 0.1 and less than or equal to 0.5, x is more than or equal to 0.7 and less than or equal to 0.9, and z is more than or equal to 0.1 and less than or equal to 0.5; the element A is one or more of Ni and Ti, the element Q is one or more of Cu, Ag, Au or Pt, and the element R is one or more of Ce, Mn, Si or Zr; the thickness of the biphase nanocrystalline soft magnetic film is 30-40 mu m, the thickness of the nanometer hexagonal boron nitride layer is 8-10 mu m, the thickness of the nanometer ZnO layer is 20-30 mu m, and the biphase nanocrystalline soft magnetic film is alpha- (Fe) with bbc structurezA1-z)aCobQcBadNano metal particles and RO2Insulating medium nano-particle composition, alpha- (Fe) of the bbc structurezA1-z)aCobQcBadNano metal particles are coated with the RO2Insulating medium nanoparticle coating, the alpha- (Fe)zA1-z)aCobQcBadThe diameter of the nano metal particles is 2 nm-5 nm, and the RO2The diameter of the insulating medium nano particles is 0.25 nm-0.5 nm.
Further, the Curie temperature Tc of the soft magnetic particle film is 260 to 280 ℃.
Further, the uniaxial anisotropy field of the soft magnetic particle film is 6.50kA/m to 8.50 kA/m.
Further, a plurality of said overlapping repeating structures are located on the upper and lower sides of said middle two-phase nano-crystalline soft magnetic thin film, said one overlapping repeating structure is a layer of said nano ZnO layer located on the upper side of a layer of said nano hexagonal boron nitride layer, said upper side of said middle two-phase nano-crystalline soft magnetic thin film is said nano hexagonal boron nitride layer, and said lower side of said middle two-phase nano-crystalline soft magnetic thin film is said nano ZnO layer.
Furthermore, one side of the outer side of the double-phase nano-crystalline soft magnetic film is provided with 2-4 overlapped repeating structures.
The invention also provides a preparation method of the anti-electromagnetic interference soft magnetic particle film, which comprises the following steps:
1) using a glass cover glass with the thickness of 0.15-0.18 mm as a substrate, placing the substrate into a solution with an anionic surfactant as a detergent, soaking for 20-30 min, cleaning for 10-15 min by using ultrasonic waves at the ultrasonic frequency of 50-80 Hz, placing the substrate into a mixed organic solvent of absolute ethyl alcohol and acetone with the volume ratio of (2:5) - (3:5), cleaning for 10-20 min at the ultrasonic frequency of 30-45 Hz, and blow-drying the substrate in hot air at the temperature of 50-60 ℃ to obtain a clean and dry substrate sheet;
2) adopting high vacuum oblique three-target co-sputtering equipment, setting the plane of the target and the horizontal plane to form a angle of 20-30 degrees, setting the distance between the target and the substrate to be 80-100 mm, filling argon gas, and subjecting a plurality of RO with the purity of 99.9 percent2The compound solid small pieces are regularly arranged in Fe with the diameter of 70 mm-80 mmz×aCobBadOn the annular etching region of the first sputtering target, adjusting the Fez×aCobBadThe sputtering power of the first sputtering target of (2) is 120W to 140W; the second sputtering target is a pure A element sputtering target, the sputtering power of the second sputtering target is adjusted to be 20-120W, and the content of the A element in the finally formed two-phase nanocrystalline soft magnetic film is further adjusted; the third sputtering target is a pure Q element sputtering target, the sputtering power of the third sputtering target is adjusted to be 20-120W, and the content of the Q element in the finally formed biphase nanocrystalline soft magnetic film is further adjusted to ensure that the ratio of the final Fe element, the final A element, the final Co element, the final Q element and the final Ba element is (zxa): ((1-z) × a): b: c: d; adjusting the RO2The amount of solid small pieces of the compound to ensure that the ratio of Fe element to R element is (z × a × (1-x)): x;
3) during the sputtering process, the pressure of the sputtering argon is adjusted to be 0.5Pa to 0.6Pa, the rotation speed of the substrate is 65rpm to 75rpm, the vacuum degree of the back bottom is 5.510-5Pa～5.8×10-5Pa; and after the sputtering is finished, obtaining the dual-phase nano-crystalline soft magnetic film, placing the nano ZnO powder and the nano hexagonal boron nitride powder in a vacuum sprayer under vacuum, and sequentially spraying the nano ZnO powder and the nano hexagonal boron nitride powder on the dual-phase nano-crystalline soft magnetic film under the pressure of 35 MPa-40 MPa to form a nano ZnO layer and a nano hexagonal boron nitride layer which are positioned at two sides of the dual-phase nano-crystalline soft magnetic film and are mutually spaced and overlapped.
Further, the flow rate of the argon gas is 30sccm to 40 sccm.
Further, the purity of the target material of the sputtering target is 99.95-99.99%.
The invention has the beneficial effects that:
1) due to the soft magnetic material Fez×aCobBadPrepared by a sputtering method, is doped with A element and Q element, and can improve Fe by utilizing A element and Q element substrate layersz×aCobBadThe soft magnetic property of the soft magnetic material is that the element A partially replaces the element Fe, and the formed Fe-Ni alloy or Fe-Ti alloy can improve the Curie temperature of the amorphous nanocrystalline two-phase soft magnetic film and improve the stability in a high-temperature environment.
2) And by adding RO2Alpha- (Fe) doped with bbc-wrapped structurezA1-z)aCobQcBadThe nano metal effectively reduces the coercive force, improves the soft magnetic performance, is beneficial to the grain refinement of the film, thereby generating exchange coupling among grains and averagely changing the magnetocrystalline anisotropy into smaller effective anisotropy; at the same time, the coercive force can be reduced to mu0MsAnd if the resistance is more than 2.5T, the resistivity is improved, the eddy current loss is effectively reduced, and the cut-off frequency of the film is improved.
3) The non-metal M element is added to promote the precursor Fez×aCobBadThe final double-phase nano-crystalline soft magnetic film can form a better nano-crystalline phase by adding a ferromagnetic transition metal element-A, so that the alpha- (Fe) with the bbc structure is formedzA1-z)aCobQcBadNano metal particles are coated with the RO2The insulating medium nano particles are wrapped, so that the final soft magnetic particle film has a disordered three-dimensional microstructure, the higher amorphous crystallization temperature is ensured, and the soft magnetic particle film can have higher stability at high temperature.
4) The symmetrical nanometer ZnO layer and the nanometer hexagonal boron nitride layer which are mutually overlapped at intervals are formed on the two sides of the middle double-phase nanometer crystal soft magnetic film, a certain electromagnetic shielding effect can be improved through the nanometer hexagonal boron nitride layer, higher resistivity is guaranteed through the nanometer ZnO layer, and then the effects of high resistivity and high electromagnetic shielding are achieved simultaneously.
Drawings
The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings. Wherein:
FIG. 1 is a schematic view of a structure of a soft magnetic particle film provided in example 1 of the present invention;
FIG. 2 is a schematic view of the structure of a soft magnetic particle film provided in example 2 of the present invention;
fig. 3 is a schematic view of the structure of a soft magnetic particle film provided in embodiment 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation of the soft magnetic particle film is carried out by adopting JGP450 type high vacuum three-target co-sputtering deposition coating equipment sold by Shenyang New blue sky vacuum technology Limited company.
Example 1
As shown in fig. 1, the anti-electromagnetic interference soft magnetic particle film provided in this embodiment is a 9-layer structure, which is a middle two-phase nano-crystalline soft magnetic film 1 and 2 overlapping repeating structures 2 located at two sides of the two-phase nano-crystalline soft magnetic film 1, and includes a nano ZnO layer 2-1 and a nano hexagonal boron nitride layer 2-2, the 2 overlapping repeating structures 2 are located at two sides of the middle two-phase nano-crystalline soft magnetic film 1, the 1 overlapping repeating structure 2 is a nano ZnO layer 2-1 located at an upper side of a nano hexagonal boron nitride layer 2-2, the upper side of the two-phase nano-crystalline soft magnetic film 1 is the nano hexagonal boron nitride layer 2-2, and the lower side of the two-phase nano-crystalline soft magnetic film 1 is the nano ZnO layer 2-1;
wherein the structural formula of the biphase nanocrystalline soft magnetic film is ((Fe)0.1Ti0.9)60Co50Cu30Ba0.5)0.3-(CeO2)0.7(ii) a Ti is a ferromagnetic transition metal element, and Cu is a noble metal element;
the thickness of the biphase nanocrystalline soft magnetic film is 30 mu m, the thickness of the nanometer hexagonal boron nitride layer is 8 mu m, the thickness of the nanometer ZnO layer is 20 mu m, and the biphase nanocrystalline soft magnetic film is alpha- (Fe) with bbc structure0.1Ti0.9)60Co50Cu30Ba0.5Nano metal particle and CeO2Insulating medium nano particle composition, bbc structure alpha- (Fe)0.1Ti0.9)60Co50Cu30Ba0.5Nano metal particle coated with CeO2Insulating dielectric nanoparticle coating, alpha- (Fe)0.1Ti0.9)60Co50Cu30Ba0.5The diameter of the nano metal particles is 2nm, CeO2The diameter of the insulating medium nano-particles is 0.25 nm.
The embodiment also provides a preparation method of the electromagnetic interference resistant soft magnetic particle film, which comprises the following steps:
1) using a glass cover glass with the thickness of 0.15mm as a substrate, placing the substrate into a solution with an anionic surfactant as a detergent, soaking for 20min, cleaning for 10min by using ultrasonic waves at the ultrasonic frequency of 50Hz, placing the substrate into an organic solvent mixed by absolute ethyl alcohol and acetone in the volume ratio of (2:5) - (3:5), cleaning for 10min at the ultrasonic frequency of 30Hz, and drying the substrate by blowing in hot air at the temperature of 50 ℃ to obtain a clean and dry substrate sheet;
2) adopting high vacuum oblique three-target co-sputtering equipment, setting the target plane and horizontal plane to form 20 degrees, and setting the target and substrateThe distance between the CeO and the CeO is 80mm, argon is filled in, the flow rate of the argon is kept to be 30sccm, and a plurality of CeO with the purity of 99.9 percent2The compound solid small pieces are regularly arranged in Fe with the diameter of 70mm6Co50Ba0.5On the annular etching region of the first sputtering target, adjusting Fe6Co50Ba0.5The sputtering power of the first sputtering target of (2) is 120W; the second sputtering target is a pure Ti sputtering target, the sputtering power of the second sputtering target is adjusted to be 20W, and the content of Ti element in the finally formed biphase nanocrystalline soft magnetic film is further adjusted; the third sputtering target is a pure Cu element sputtering target, the sputtering power of the third sputtering target is adjusted to be 20W, the content of the M element in the finally formed dual-phase nanocrystalline soft magnetic film is further adjusted, and the ratio of the final Fe element, the Ti element, the Co element, the Cu element and the Ba element is ensured to be 6:54:50:30: 0.5; adjusting CeO2The number of compound solid small pieces ensures that the ratio of Fe element to Ce element is 1.8: 0.7;
the target material purity of the first sputtering target is 99.99 percent, the target material purity of the second sputtering target is 99.96 percent, and the target material purity of the third sputtering target is 99.97 percent;
3) during sputtering, the pressure of the sputtering argon is adjusted to be 0.5Pa, the rotation speed of the substrate is 65rpm, and the vacuum degree of the back bottom is 5.5 multiplied by 10-5Pa; and after the sputtering is finished, obtaining a dual-phase nano-crystalline soft magnetic film, placing nano ZnO powder and nano hexagonal boron nitride powder in a vacuum sprayer under vacuum, and sequentially spraying the nano ZnO powder and the nano hexagonal boron nitride powder on the dual-phase nano-crystalline soft magnetic film under the pressure of 35MPa to form a nano ZnO layer and a nano hexagonal boron nitride layer which are positioned on two sides of the dual-phase nano-crystalline soft magnetic film and are mutually spaced and overlapped.
Through tests, the Curie temperature Tc of the soft magnetic particle film provided by the embodiment is 260 ℃, the uniaxial anisotropy field is 6.50kA/m, and the anti-electromagnetic interference rate reaches 98.55%.
Example 2
As shown in fig. 2, for the soft magnetic particle film for resisting electromagnetic interference provided in this embodiment, the soft magnetic particle film is a 13-layer structure, and is a middle two-phase nano-crystalline soft magnetic film 1 and 3 overlapping repeating structures 2 located at two sides of the two-phase nano-crystalline soft magnetic film 1, where 1 overlapping repeating structure 2 includes a nano ZnO layer 2-1 and a nano hexagonal boron nitride layer 2-2, 3 overlapping repeating structures 2 are located at upper and lower sides of the middle two-phase nano-crystalline soft magnetic film 1, 1 overlapping repeating structure 2 is a nano ZnO layer 2-1 located at an upper side of the nano hexagonal boron nitride layer 2-2, the upper side of the middle two-phase nano-crystalline soft magnetic film 1 is the nano hexagonal boron nitride layer 2-2, and the lower side of the middle two-phase nano-crystalline soft magnetic film 1 is the nano ZnO layer 2-1;
wherein the structural formula of the biphase nanocrystalline soft magnetic film is ((Fe)0.5Ni0.5)30Co70Ag10Ba0.1)0.1-(MnO2)0.9(ii) a Ni element is ferromagnetic transition metal element, Ag element is noble metal element; the thickness of the biphase nanocrystalline soft magnetic film is 40 mu m, the thickness of the nanometer hexagonal boron nitride layer is 10 mu m, the thickness of the nanometer ZnO layer is 30 mu m, and the biphase nanocrystalline soft magnetic film is alpha- (Fe) with bbc structure0.5Ni0.5)30Co70Ag10Ba0.1Nano metal particles and RO2Insulating medium nano particle composition, bbc structure alpha- (Fe)0.5Ni0.5)30Co70Ag10Ba0.1MnO of nano metal particles2Insulating dielectric nanoparticle coating, alpha- (Fe)0.5Ni0.5)30Co70Ag10Ba0.1The diameter of the nano metal particles is 5nm, MnO2The diameter of the insulating medium nano-particles is 0.5 nm.
The embodiment also provides a preparation method of the electromagnetic interference resistant soft magnetic particle film, which comprises the following steps:
1) using a glass cover glass with the thickness of 0.18mm as a substrate, placing the substrate into a solution with an anionic surfactant as a detergent, soaking for 30min, cleaning for 15min by using ultrasonic waves at the ultrasonic frequency of 80Hz, placing the substrate into an absolute ethyl alcohol and acetone mixed organic solvent with the volume ratio of 3:5, cleaning for 20min at the ultrasonic frequency of 45Hz, and blow-drying the substrate in hot air at the temperature of 60 ℃ to obtain a clean and dry substrate sheet;
2) adopting high vacuum oblique three-target co-sputtering equipment, setting the target plane and horizontal plane to form 30 DEG, and setting the distance between the target and the substrateIntroducing argon gas into the reactor at a flow rate of 40sccm when the distance is 100mm, and adding MnO with a purity of 99.9%2The compound solid small pieces are regularly arranged in Fe with the diameter of 80mm15Co70Ba0.1On the annular etching region of the first sputtering target, adjusting Fe15Co70Ba0.1The sputtering power of the first sputtering target of (2) is 140W; the second sputtering target is a pure Ni element sputtering target, the sputtering power of the second sputtering target is adjusted to be 120W, and further the content of the Ni element in the finally formed biphase nanocrystalline soft magnetic film is adjusted; the third sputtering target is a pure Ag element sputtering target, the sputtering power of the third sputtering target is adjusted to be 120W, the content of the Ag element in the finally formed dual-phase nanocrystalline soft magnetic film is further adjusted, and the ratio of the Fe element, the Ni element, the Co element, the Ag element and the Ba element is ensured to be 15:15:70:10: 0.1; adjustment of MnO2The number of solid small pieces of the compound ensures that the ratio of Fe element to Mn element is 1.5: 0.9;
the target material purity of the first sputtering target is 99.95%, the target material purity of the second sputtering target is 99.975%, and the target material purity of the third sputtering target is 99.98%;
3) during sputtering, the pressure of the sputtering argon is adjusted to be 0.6Pa, the rotation speed of the substrate is 75rpm, and the vacuum degree of the back bottom is 5.8 multiplied by 10-5Pa; and after the sputtering is finished, obtaining a dual-phase nano-crystalline soft magnetic film, placing nano ZnO powder and nano hexagonal boron nitride powder in a vacuum sprayer under vacuum, and sequentially spraying the nano ZnO powder and the nano hexagonal boron nitride powder on the dual-phase nano-crystalline soft magnetic film under the pressure of 40MPa to form a nano ZnO layer and a nano hexagonal boron nitride layer which are positioned on two sides of the dual-phase nano-crystalline soft magnetic film and are mutually spaced and overlapped.
Through tests, the Curie temperature Tc of the soft magnetic particle film provided by the embodiment is 280 ℃, the uniaxial anisotropy field is 8.50 kA/m, and the anti-electromagnetic interference rate is 99.65%.
Example 3
As shown in fig. 3, the soft magnetic particle film for resisting electromagnetic interference provided in this embodiment is characterized in that the soft magnetic particle film has a 16-layer structure, which is a middle two-phase nano-crystalline soft magnetic film 1 and 4 overlapping repeating structures 2 located at two sides of the two-phase nano-crystalline soft magnetic film 1, where the 1 overlapping repeating structure 2 includes a nano ZnO layer 2-1 and a nano hexagonal boron nitride layer 2-2, the 4 overlapping repeating structures 2 are located at two upper and lower sides of the middle two-phase nano-crystalline soft magnetic film 1, the 1 overlapping repeating structure 2 is a nano ZnO layer 2-1 located at an upper side of the nano hexagonal boron nitride layer 2-2, the upper side of the middle two-phase nano-crystalline soft magnetic film 1 is the nano hexagonal boron nitride layer 2-2, and the lower side of the middle two-phase nano-crystalline soft magnetic film 1 is the nano ZnO layer 2-1;
wherein the structural formula of the biphase nanocrystalline soft magnetic film is ((Fe)0.3Ti0.7)40Co60Pt20Ba0.3)0.2-(SiO2)0.8(ii) a Ti element is ferromagnetic transition metal element, Pt element is noble metal element; the thickness of the biphase nanocrystalline soft magnetic film is 35 mu m, the thickness of the nanometer hexagonal boron nitride layer is 9 mu m, the thickness of the nanometer ZnO layer is 25 mu m, and the biphase nanocrystalline soft magnetic film is alpha-Fe with bbc structure0.3Ti0.7)40Co60Pt20Ba0.3Nano metal particles and SiO2Insulating dielectric nanoparticle composition, bbc structure alpha-Fe0.3Ti0.7)40Co60Pt20Ba0.3Nano metal particle coated with SiO2Insulating dielectric nanoparticle coated, alpha-Fe0.3Ti0.7)40Co60Pt20Ba0.3The diameter of the nano metal particles is 3.5nm, SiO2The diameter of the insulating medium nano-particles is 0.35 nm.
The embodiment provides a preparation method of the above electromagnetic interference resistant soft magnetic particle film, which includes the following steps:
1) using a glass cover glass with the thickness of 0.17mm as a substrate, placing the substrate into a solution with an anionic surfactant as a detergent, soaking for 25min, cleaning for 13min by using ultrasonic waves at the ultrasonic frequency of 65Hz, placing the substrate into an absolute ethyl alcohol and acetone mixed organic solvent with the volume ratio of 1:2, cleaning for 15min at the ultrasonic frequency of 40Hz, and blow-drying the substrate under hot air at the temperature of 55 ℃ to obtain a clean and dry substrate sheet;
2) adopting high vacuum oblique three-target co-sputtering equipment, setting the plane of the target and the horizontal plane to form an angle of 25 degrees, and setting the target and the substrate betweenThe distance between the two parts is 90mm, argon is filled in, the flow rate of the argon is kept to be 35sccm, and a plurality of RO with the purity of 99.9 percent are added2The solid compound flakes are regularly arranged in 75mm diameter Fez×aCobBadOn the annular etching region of the first sputtering target, adjusting Fez×aCobBadThe sputtering power of the first sputtering target of (1) is 130W; the second sputtering target is a pure Ti sputtering target, the sputtering power of the second sputtering target is adjusted to 70W, and the content of Ti element in the finally formed biphase nanocrystalline soft magnetic film is further adjusted; the third sputtering target is a pure Pt element sputtering target, the sputtering power of the third sputtering target is adjusted to be 70W, the content of the Pt element in the finally formed dual-phase nanocrystalline soft magnetic film is further adjusted, and the ratio of the final Fe element, the Ti element, the Co element, the Pt element and the Ba element is ensured to be 12:28:60:20: 0.3; adjusting RO2The number of solid small pieces of the compound ensures that the ratio of Fe element to R element is 3: 1;
the target purity of the first sputtering target was 99.965%, the target purity of the second sputtering target was 99.985%, and the target purity of the third sputtering target was 99.973%;
3) during sputtering, the pressure of sputtering argon is adjusted to 0.55Pa, the rotation speed of the substrate is 71rpm, and the vacuum degree of the back substrate is 5.67X 10-5Pa; and after the sputtering is finished, obtaining a dual-phase nano-crystalline soft magnetic film, placing nano ZnO powder and nano hexagonal boron nitride powder in a vacuum sprayer under vacuum, and sequentially spraying the nano ZnO powder and the nano hexagonal boron nitride powder on the dual-phase nano-crystalline soft magnetic film under the pressure of 38MPa to form a nano ZnO layer and a nano hexagonal boron nitride layer which are positioned on two sides of the dual-phase nano-crystalline soft magnetic film and are mutually spaced and overlapped.
Through tests, the Curie temperature Tc of the soft magnetic particle film provided by the embodiment is 275 ℃, the uniaxial anisotropy field is 7.35kA/m, and the anti-electromagnetic interference rate reaches 99.45%.
While the invention has been described with reference to a preferred embodiment, various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the technical features mentioned in the embodiments can be combined in any way as long as there is no structural conflict. The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention. It is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.

Claims (8)

1. An anti-electromagnetic interference soft magnetic particle film, characterized in that the soft magnetic particle film is a multilayer structure, which is a middle dual-phase nano-crystalline soft magnetic film (1) and a plurality of overlapping repeating structures (2) positioned at the upper side and a plurality of overlapping repeating structures (2) positioned at the lower side of the dual-phase nano-crystalline soft magnetic film (1), and the one overlapping repeating structure (2) comprises a nano-ZnO layer (2-1) and a nano-hexagonal boron nitride layer (2-2);
the structural formula of the biphase nanocrystalline soft magnetic film is ((Fe)zA1-z)aCobQcBad)1-x-(RO2)xWherein a is more than or equal to 30 and less than or equal to 60, b is more than or equal to 50 and less than or equal to 70, c is more than or equal to 10 and less than or equal to 30, d is more than or equal to 0.1 and less than or equal to 0.5, x is more than or equal to 0.7 and less than or equal to 0.9, and z is more than or equal to 0.1 and less; the element A is one or more of Ni and Ti, the element Q is one or more of Cu, Ag, Au or Pt, and the element R is one or more of Ce, Mn, Si or Zr; the thickness of the biphase nanocrystalline soft magnetic film is 30-40 mu m, the thickness of the nanometer hexagonal boron nitride layer is 8-10 mu m, the thickness of the nanometer ZnO layer is 20-30 mu m, and the biphase nanocrystalline soft magnetic film is alpha- (Fe) with bbc structurezA1-z)aCobQcBadNano metal particles and RO2Insulating medium nano-particle composition, alpha- (Fe) of the bbc structurezA1-z)aCobQcBadNano metal particle quilt coverThe RO2Insulating medium nanoparticle coating, the alpha- (Fe)zA1-z)aCobQcBadThe diameter of the nano metal particles is 2 nm-5 nm, and the RO2The diameter of the insulating medium nano particles is 0.25 nm-0.5 nm.
2. The soft magnetic particle film against electromagnetic interference according to claim 1, wherein the Curie temperature Tc of said soft magnetic particle film is 260 ℃ to 280 ℃.
3. The soft magnetic particle film against electromagnetic interference according to claim 1, wherein said soft magnetic particle film has a uniaxial anisotropy field of 6.50kA/m to 8.50 kA/m.
4. The soft magnetic particle film against electromagnetic interference according to claim 1, wherein a plurality of said overlapping repeating structures (2) are located on the upper and lower sides of said middle dual-phase nano-crystalline soft magnetic film (1), said one overlapping repeating structure (2) is a layer of said nano ZnO layer (2-1) located on the upper side of a layer of said nano hexagonal boron nitride layer (2-2), said middle dual-phase nano-crystalline soft magnetic film (1) is an upper side of said nano hexagonal boron nitride layer (2-2), and said middle dual-phase nano-crystalline soft magnetic film (1) is an underside of said nano ZnO layer (2-1).
5. An anti-electromagnetic interference soft magnetic particle film according to claim 1, characterized in that said bi-phase nano-crystalline soft magnetic thin film (1) has 2-4 of said overlapping repeating structures (2) on the outer side.
6. The method for preparing an anti-electromagnetic interference soft magnetic particle film according to any one of claims 1 to 5, comprising the steps of:
1) using a glass cover glass with the thickness of 0.15-0.18 mm as a substrate, placing the substrate into a solution with an anionic surfactant as a detergent, soaking for 20-30 min, cleaning for 10-15 min by using ultrasonic waves at the ultrasonic frequency of 50-80 Hz, placing the substrate into a mixed organic solvent of absolute ethyl alcohol and acetone with the volume ratio of (2:5) - (3:5), cleaning for 10-20 min at the ultrasonic frequency of 30-45 Hz, and blow-drying the substrate in hot air at the temperature of 50-60 ℃ to obtain a clean and dry substrate sheet;
2) adopting high vacuum oblique three-target co-sputtering equipment, setting the plane of the target and the horizontal plane to form a angle of 20-30 degrees, setting the distance between the target and the substrate to be 80-100 mm, filling argon gas, and subjecting a plurality of RO with the purity of 99.9 percent2The compound solid small pieces are regularly arranged in Fe with the diameter of 70 mm-80 mmz×aCobBadOn the annular etching region of the first sputtering target, adjusting the Fez× aCobBadThe sputtering power of the first sputtering target of (2) is 120W to 140W; the second sputtering target is a pure A element sputtering target, the sputtering power of the second sputtering target is adjusted to be 20-120W, and the content of the A element in the finally formed two-phase nanocrystalline soft magnetic film is further adjusted; the third sputtering target is a pure Q element sputtering target, the sputtering power of the third sputtering target is adjusted to be 20-120W, and the content of the Q element in the finally formed biphase nanocrystalline soft magnetic film is further adjusted to ensure that the ratio of the final Fe element, the final A element, the final Co element, the final Q element and the final Ba element is (zxa): ((1-z) × a): b: c: d; adjusting the RO2The amount of solid small pieces of the compound to ensure that the ratio of Fe element to R element is (z × a × (1-x)): x;
3) in the sputtering process, the pressure of the sputtering argon is adjusted to be 0.5 Pa-0.6 Pa, the rotation speed of the substrate is 65 rpm-75 rpm, and the vacuum degree of the back substrate is 5.5 multiplied by 10-5Pa～5.8×10-5Pa; and after the sputtering is finished, obtaining the dual-phase nano-crystalline soft magnetic film, placing the nano ZnO powder and the nano hexagonal boron nitride powder in a vacuum sprayer under vacuum, and sequentially spraying the nano ZnO powder and the nano hexagonal boron nitride powder on the dual-phase nano-crystalline soft magnetic film under the pressure of 35 MPa-40 MPa to form a nano ZnO layer and a nano hexagonal boron nitride layer which are positioned at two sides of the dual-phase nano-crystalline soft magnetic film and are mutually spaced and overlapped.
7. The method for preparing an anti-electromagnetic interference soft magnetic particle film according to claim 6, wherein the flow rate of argon gas is 30sccm to 40 sccm.
8. The method according to claim 6, wherein the purity of the target material of the sputtering target is 99.95-99.99%.
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Denomination of invention: A Soft Magnetic Particle Film with Anti electromagnetic Interference and Its Preparation Method

Effective date of registration: 20221223

Granted publication date: 20210820

Pledgee: Fuyang Erlijing Sub branch of China Construction Bank Corp.

Pledgor: ANHUI ZHICI NEW MATERIAL TECHNOLOGY Co.,Ltd.

Registration number: Y2022980028904