CN114150236A - Iron-based amorphous alloy film, preparation method thereof, electromagnetic shielding film and equipment applying iron-based amorphous alloy film - Google Patents
Iron-based amorphous alloy film, preparation method thereof, electromagnetic shielding film and equipment applying iron-based amorphous alloy film Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 74
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- 238000003723 Smelting Methods 0.000 claims description 4
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/11—Making amorphous alloys
-
- 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
- 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
- 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
- C23C14/14—Metallic material, boron or silicon
-
- 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
- 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
- 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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses an iron-based amorphous alloy film, which comprises the following components in percentage by mass: fe is more than or equal to 70 wt% and less than or equal to 90 wt%, Co is more than or equal to 0 wt% and less than or equal to 6 wt%, Si is more than or equal to 1 wt% and less than or equal to 4 wt%, B is more than or equal to 1 wt% and less than or equal to 3 wt%, Ni is more than 0.2 and less than or equal to 20 wt%, Mo is more than or equal to 0 and less than 6 wt%, and C is more than or equal to 0 and less than or equal to 3 wt%. A preparation method of an iron-based amorphous alloy film is a magnetron sputtering process, and the iron-based amorphous alloy film prepared by the process can be prepared with corresponding electromagnetic shielding films and equipment; the iron-based amorphous alloy thin film prepared by adopting the chemical component (mass percentage) range and the magnetron sputtering process has the beneficial technical effect of excellent comprehensive magnetic performance, and the electromagnetic shielding film and the equipment prepared by utilizing the iron-based amorphous alloy meet the application requirement of an electronic shielding material with high performance requirement.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to an iron-based amorphous alloy film, a preparation method thereof, an electromagnetic shielding film and equipment applying the iron-based amorphous alloy film.
Background
The amorphous soft magnetic materials on the market at present mainly comprise iron-based, cobalt-based, nickel-based and other amorphous alloys and nanocrystalline alloys. The iron-based amorphous material has the characteristics of high magnetic permeability, low coercive force and low loss, so that the iron-based amorphous material becomes an excellent soft magnetic material. With the development of science and technology, especially the rapid development of information technology, various industries will put forward higher and higher requirements on various electronic devices, the trend of miniaturization, high sensitivity, fast response and high stability will be the future, and iron-based amorphous materials will be widely applied in the fields of industrial automation, automotive electronics, information technology, medical instruments and the like.
The characteristics of low loss, low coercive force, high magnetic permeability and high remanence of the iron-based amorphous alloy enable the iron-based amorphous alloy to be widely applied to the field of electronic equipment. In order to further meet the requirements of the field of electronic equipment on the iron-based amorphous alloy, the magnetic performance of the iron-based amorphous alloy needs to be further improved.
At present, the amorphous magnetic film is mostly prepared by adopting a process of depositing an amorphous Ni-based alloy on a high-conductivity metal foil by a chemical plating/electroplating deposition technology, the chemical plating/electroplating deposition technology is easy to cause environmental pollution, and the selection of alloy components is limited by requirements; the magnetron sputtering is adopted to prepare the amorphous magnetic film, so that the selection of the components of the alloy film is wide and the alloy film is environment-friendly.
Electromagnetic shielding is an effective means for controlling electromagnetic interference, and electromagnetic shielding materials are important tools for electromagnetic shielding. Conventional metals and metal matrix composites are the most commonly used electromagnetic shielding materials. According to the strength of the electric conduction and magnetic conduction capability of the metal material, the metal material is respectively used for shielding high-frequency or low-frequency electromagnetic waves. High-conductivity metal materials such as copper, aluminum, silver, and the like are generally used for shielding high-frequency electromagnetic waves. The electrostatic field and the low frequency magnetic field are usually shielded by high permeability materials such as pure iron, silicon steel, permalloy. However, the traditional metal material has the problems of large density, heavy weight, poor flexibility, narrow corresponding frequency bandwidth, limited shielding effectiveness and the like.
At present, due to different functional requirements of electronic products and devices, electromagnetic waves generated by high-frequency oscillation contain various complicated high-low frequency bands, and the conventional electromagnetic shielding material is difficult to solve the complicated electromagnetic compatibility problem, so that a novel electromagnetic shielding material with more excellent performance needs to be developed.
Disclosure of Invention
The invention provides an iron-based amorphous alloy film, a preparation method thereof, an electromagnetic shielding film and equipment using the iron-based amorphous alloy film to overcome the defects of the prior art.
The iron-based amorphous alloy film comprises the following components in percentage by mass: fe is more than or equal to 70 wt% and less than or equal to 90 wt%, Co is more than or equal to 0 wt% and less than or equal to 6 wt%, Si is more than or equal to 1 wt% and less than or equal to 4 wt%, B is more than or equal to 1 wt% and less than or equal to 3 wt%, Ni is more than 0.2 and less than or equal to 20 wt%, Mo is more than or equal to 0 and less than 6 wt%, and C is more than or equal to 0 and less than or equal to 3 wt%.
Further, the composition also comprises C, P, S elements, wherein the mass percent of each element is as follows: fe is more than or equal to 70 wt% and less than or equal to 90 wt%, Co is more than or equal to 0 wt% and less than or equal to 6 wt%, Si is more than or equal to 1 wt% and less than or equal to 4 wt%, B is more than or equal to 1 wt% and less than or equal to 3 wt%, Ni is more than 0.2 and less than or equal to 20 wt%, Mo is more than or equal to 0 and less than or equal to 6 wt%, C is more than or equal to 0 and less than or equal to 3 wt%, X is less than or equal to 5 wt%, and X is any one or more of C, P, S elements.
A preparation method for preparing the iron-based amorphous alloy film comprises the following steps:
s1, smelting the raw materials to obtain a master alloy, and finely processing the master alloy to obtain an iron-based alloy target; the raw materials comprise Fe, Co, B, Si, Ni, Mo and C, and the mass percentages of the elements are as follows: fe is more than or equal to 70 wt% and less than or equal to 90 wt%, Co is more than or equal to 0 wt% and less than or equal to 6 wt%, Si is more than or equal to 1 wt% and less than or equal to 4 wt%, B is more than or equal to 1 wt% and less than or equal to 3 wt%, Ni is more than 0.2 and less than or equal to 20 wt%, Mo is more than or equal to 0 and less than 6 wt%, C is more than or equal to 0 and less than or equal to 3 wt%;
s2, enabling the temperature of the substrate to be lower than 80 ℃, placing the substrate which is connected with the ground in parallel on the side surface of the iron-based alloy target, and keeping a distance L between the substrate and the iron-based alloy target, wherein the L is within a range of 2-10 cm; depositing on a substrate by adopting a magnetron sputtering method to obtain an amorphous iron-based amorphous alloy;
s3, keeping the power of the pulse power supply within the range of 2-10 kw, and depositing metal on the substrate for a time T to form the iron-based amorphous alloy film on the substrate.
Further, in the step S1, the thickness of the iron-based alloy target is 1 to 6 mm.
Further, in the step S2 and the step S3, the deposition temperature of the substrate is less than 120 ℃ during magnetron sputtering; the working gas adopted by magnetron sputtering is Ar, and the vacuum degree after Ar is introduced is 1 multiplied by 10-1～5×10-1Pa; the working current of the magnetron sputtering is within the range of 4-12A, the linear speed of the coating film is 0.5-5 m/min, and the sputtering time T is 5-120 min.
Further, in the step S2 and the step S3, the working temperature of the working chamber is maintained at 25 ℃ to 100 ℃ during plating.
Further, the thickness of the iron-based amorphous alloy film is 20-2000 nm.
Further, in step S1, any one or more of C, P, S elements are prepared into a pure element or mixed element target, and the mass ratio of the iron-based alloy target to the pure element or mixed element target is 10: 1 to form a combined target material; in step S2, the temperature of the substrate is made to be less than 80 ℃, and the substrate connected to the ground is placed in parallel on the side surface of the combined target, and the distance L between the substrate and the combined target is kept, wherein L is in the range of 2-10 cm, and the amorphous iron-based amorphous alloy is obtained by depositing on the substrate by a magnetron sputtering method.
Further, the thickness of the combined target is 1-6 mm.
Further, in the step S2 and the step S3, the deposition temperature of the substrate is less than 120 ℃ during magnetron sputtering; the working gas adopted by magnetron sputtering is Ar, and the vacuum degree after Ar is introduced is 1 multiplied by 10-1～5×10-1Pa; the working current of the magnetron sputtering is within the range of 4-12A, the linear speed of the coating film is 0.5-5 m/min, and the sputtering time T is 5-120 min.
Further, in the step S2 and the step S3, the working temperature of the working chamber is maintained at 25 ℃ to 100 ℃ during plating.
Further, the thickness of the iron-based amorphous alloy film is 20-2000 nm.
The electromagnetic shielding film comprises a carrier layer, a magnetic conduction layer and a protective layer which are sequentially arranged, wherein the magnetic conduction layer is the iron-based amorphous alloy film.
Furthermore, the magnetic conduction layer is formed by sequentially arranging a plurality of iron-based amorphous alloy films.
Further, any one or more of a C fiber layer, a P fiber layer and an S fiber layer are arranged between the adjacent magnetic conduction layers.
Further, a conducting layer is arranged between the magnetic conduction layer and the protective layer, and the conducting layer is any one of a metal shielding layer, a carbon nanotube shielding layer and a graphene shielding layer or is formed by sequentially arranging any multiple of the metal shielding layer, the carbon nanotube shielding layer and the graphene shielding layer.
Further, the metal shielding layer comprises a single metal shielding layer and/or an alloy shielding layer; the single metal shielding layer is made of any one of aluminum, titanium, zinc, iron, nickel, chromium, cobalt, copper, silver and gold, and the alloy shielding layer is made of any two or more of aluminum, titanium, zinc, iron, nickel, chromium, cobalt, copper, silver and gold.
Further, the adjacent conducting layers and the magnetic conduction layers are connected through one or more modes of chemical plating, PVD, CVD, evaporation plating, sputtering plating, electroplating or composite plating.
Further, the protective layer and the carrier layer are any one of a PPS film layer, a PEN film layer, a polyester film layer, a polyimide film layer, a film layer formed after epoxy resin ink is cured, a film layer formed after polyurethane ink is cured, a film layer formed after modified acrylic resin is cured, and a film layer formed after polyimide resin is cured.
An apparatus comprising the above electromagnetic shielding film.
The invention has the beneficial effects that:
the invention has the beneficial effects that:
the iron-based amorphous alloy film prepared by adopting the chemical component (mass percentage) range and the magnetron sputtering process has the beneficial technical effects that the magnetic performance is improved, the magnetic conductivity and the shielding effectiveness of the iron-based amorphous alloy film are effectively improved due to the fact that microalloying of the amorphous alloy is a method for improving the magnetic performance of the material, and the NI element is added to change the atom arrangement and the interaction among atoms, so that the application requirement of an electronic shielding material with high performance requirement is met by utilizing the electromagnetic shielding film prepared by the iron-based amorphous alloy film. Meanwhile, the iron-based amorphous alloy film is used as an electromagnetic shielding film made of the magnetic conduction layer, has high magnetic conductivity, can realize better shielding efficiency under different electromagnetic frequencies, has good magnetic shielding effect in a high-frequency electromagnetic field (100 kHz) and a low-frequency magnetic field (below 100kHz), and has wider frequency application.
On the other hand, because C, P, S element has better flexibility, C, P, S element is introduced into the iron-based amorphous alloy, the arrangement of atoms is improved, the atomic bond state and the interatomic bonding force are changed, the internal defects of the alloy are improved, the flexibility of the iron-based amorphous alloy can be effectively improved, and the iron-based amorphous alloy can be well applied to equipment with higher requirements on flexibility, such as flexible circuit boards and the like.
Drawings
FIG. 1 is a schematic view showing the structure of an electromagnetic shielding film according to embodiments 12 to 20 of the present invention;
fig. 2 is a schematic structural view of an electromagnetic shielding film in embodiment 21 of the present invention;
FIG. 3 is a schematic view showing the structure of an electromagnetic shielding film according to embodiment 22 of the present invention;
fig. 4 is a schematic structural view of an electromagnetic shielding film in embodiment 23 of the present invention;
FIG. 5 is an XRD test pattern of the Fe-based amorphous alloy in example 1 of the present invention;
FIG. 6 is XRD test picture of Fe-based amorphous alloy in example 8 of the present invention.
Description of reference numerals: 1. a protective layer; 2. a conductive layer; 3. a magnetically conductive layer; 4. a carrier layer; and 5.C fiber layer.
Detailed Description
In order to make the technical solution, objects and advantages of the present invention more apparent, the following examples further illustrate the present invention.
Example 1:
this example 1 provides an Fe-based amorphous alloy thin film, the chemical composition expression of which is Fe69Ni14B13Si4The XRD test pattern of the fe-based amorphous alloy thin film is shown in fig. 5.
Example 2
This example 2 provides a method for preparing the fe-based amorphous alloy thin film of example 1. Calculating the weight ratio of Fe, Ni, B and Si according to the atomic ratio of the chemical formula, and further calculating the weight of each raw material required by each element added; and then calculating the weight of each required raw material, wherein the preparation method comprises the following specific steps:
s1, smelting the calculated weight of the raw materials to obtain Fe69Ni14B13Si4A master alloy;
s2, mixing Fe69Ni14B13Si4Cutting, polishing and grinding the master alloy according to the specification and shape of the target to obtain Fe69Ni14B13Si4Alloying the target material;
s3, Fe obtained in the previous step69Ni14B13Si4Cutting the alloy target with the shape specification of 110 multiplied by 700 multiplied by 6 mm;
s4, selecting a substrate made of a flexible insulating material, and cutting the Fe obtained in the previous step69Ni14B13Si4Placing the alloy target material and the flexible insulating substrate into a working cavity, arranging a refrigerating device below the flexible insulating substrate, and enabling the temperature of the substrate to be lower than 80 ℃ by adopting a refrigerating means;
s5, holding Fe69Ni14B13Si4The distance between the alloy target and the flexible insulating substrate is 5.5cm, and the vacuum of the chamber to be prepared reaches 5.0 multiplied by 10-5Introducing Ar gas when Pa;
s6, when the vacuum degree of the preparation chamber is adjusted to 2.2X 10-1When Pa, adjusting air pressure to make it glow;
s7, adjusting the voltage of a pulse power supply to 420V, the current to 6A and the linear speed of the coating film advancing to 1m/min, and carrying out metal deposition for a time T on the flexible insulating substrate to obtain Fe69Ni14B13Si4An amorphous alloy thin film.
In the preparation method, the sputtering time T is 5-50 min, and Fe can be controlled by adjusting the sputtering time69Ni14B13Si4Thickness of the amorphous alloy thin film.
Example 3:
this example 3 provides an Fe-based amorphous alloy thin film, the chemical composition expression of which is Fe76Ni4B13Si4C3。
Example 4:
this example 4 provides an Fe-based amorphous alloy thin film with a chemical composition expressed as Fe74Ni4B13Si4C3Mo2。
Example 5:
example 5 provides an Fe-based amorphous alloy thin filmThe chemical composition expression of the alloy film is Fe69Ni12B13Si4Mo2。
Example 6:
this example 6 provides an Fe-based amorphous alloy thin film, the chemical composition expression of which is Fe69Ni7Co3B13Si4Mo2.5。
Example 7:
example 7 provides an Fe-based amorphous alloy thin film with a chemical composition expressed as Fe68Ni6.5Co3B13Si4C3Mo2.5。
Example 8:
this example 8 provides an Fe-based amorphous alloy thin film, the chemical composition expression of which is Fe62.8Ni12.7B11.8Si3.6S9.1The XRD test pattern of the fe-based amorphous alloy thin film is shown in fig. 6.
Since the S element has a good flexibility, the flexibility of the fe-based amorphous alloy can be improved by introducing the S element into the fe-based amorphous alloy in this embodiment, so that the fe-based amorphous alloy can be well applied to devices such as flexible circuit boards, which have a high requirement for flexibility.
Example 9
This example 9 provides a method for preparing the fe-based amorphous alloy thin film of example 8. Firstly, preparing a chemical composition with an expression of Fe69Ni14B13Si4The iron-based alloy target material calculates the weight ratio of Fe, Ni, B and Si according to the atomic ratio of the chemical formula, and further calculates the weight of each raw material required by each element added to the iron-based alloy target material; and then calculating the weight of each required raw material, wherein the preparation method comprises the following specific steps:
s1, smelting the calculated weight of the raw materials to obtain Fe69Ni14B13Si4A master alloy;
s2, mixing Fe69Ni14B13Si4Cutting, polishing and grinding the master alloy according to the specification and shape of the target to obtain Fe69Ni14B13Si4Alloying the target material;
s3, preparing the S element into a pure S target material;
s4, mixing the iron-based alloy target obtained in the step S2 and the pure S target obtained in the step S3 according to the mass ratio of 10: 1 to form a combined target material;
s5, cutting the combined target material obtained in the previous step into a cylindrical combined target material;
s4, selecting a substrate made of a flexible insulating material, placing the combined target material cut in the previous step and the flexible insulating substrate into a working cavity, arranging a refrigerating device below the flexible insulating substrate, and enabling the temperature of the substrate to be lower than 80 ℃ by adopting a refrigerating method;
s5, keeping the distance between the combined target and the flexible insulating substrate to be 5.5cm, and keeping the vacuum of the chamber to be prepared to be 5.0 multiplied by 10-5Introducing Ar gas when Pa;
s6, when the vacuum degree of the preparation chamber is adjusted to 2.2X 10-1When Pa, adjusting air pressure to make it glow;
s7, adjusting the voltage of a pulse power supply to 420V, the current to 6A and the linear speed of the coating film advancing to 1m/min, and carrying out metal deposition for a time T on the flexible insulating substrate to obtain Fe62.8Ni12.7B11.8Si3.6S9.1An amorphous alloy thin film.
In the preparation method, the sputtering time T is 5-50 min, and Fe can be controlled by adjusting the sputtering time62.8Ni12.7B11.8Si3.6S9.1Thickness of the amorphous alloy thin film.
Example 10:
this example 10 provides an Fe-based amorphous alloy thin film, the chemical composition expression of which is Fe62.8Ni12.7B11.8Si3.6C9.1。
Example 11:
this example 11 provides an Fe-based amorphous alloy thin film, which is made of Fe-based amorphous alloyThe chemical composition expression of the gold film is Fe62.8Ni12.7B11.8Si3.6P9.1。
Example 12:
this example 12 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film of example 1 is selected as a magnetic conductive layer of the electromagnetic shielding film, and a chemical expression of the iron-based amorphous alloy thin film of example 1 is Fe69Ni14B13Si4. In this embodiment, the electromagnetic shielding film is sequentially arranged with a protective layer, a magnetic conductive layer and a carrier layer, and the structure thereof is as shown in fig. 1.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe69Ni14B13Si4The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 13:
this example 13 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film of example 3 is selected as a magnetic conductive layer of the electromagnetic shielding film, and a chemical expression of the iron-based amorphous alloy thin film of example 3 is Fe76Ni4B13Si4C3. In this embodiment, the electromagnetic shielding film is sequentially arranged with a protective layer, a magnetic conductive layer and a carrier layer, and the structure thereof is as shown in fig. 1.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe76Ni4B13Si4C3The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 14:
this example 14 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film of example 4 is selected as a magnetic conductive layer of the electromagnetic shielding film, and a chemical expression of the iron-based amorphous alloy thin film of example 4 is Fe74Ni4B13Si4C3Mo2. In this embodiment, the electromagnetic shielding film is sequentially arranged with a protective layer, a magnetic conductive layer and a carrier layer, and the structure thereof is as shown in fig. 1.
In this embodiment, the magnetic conductive layer is selectedChemical expression is Fe74Ni4B13Si4C3Mo2The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 15:
this example 15 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film of example 5 is selected as a magnetic conductive layer of the electromagnetic shielding film, and a chemical expression of the iron-based amorphous alloy thin film of example 5 is Fe69Ni12B13Si4Mo2. In this embodiment, the electromagnetic shielding film is sequentially arranged with a protective layer, a magnetic conductive layer and a carrier layer, and the structure thereof is as shown in fig. 1.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe69Ni12B13Si4Mo2The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 16:
this example 16 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film of example 6 is selected as a magnetic conductive layer of the electromagnetic shielding film, and a chemical expression of the iron-based amorphous alloy thin film of example 6 is Fe69Ni7Co3B13Si4Mo2.5. In this embodiment, the electromagnetic shielding film is sequentially arranged with a protective layer, a magnetic conductive layer and a carrier layer, and the structure thereof is as shown in fig. 1.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe69Ni7Co3B13Si4Mo2.5The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 17:
this example 17 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film of example 7 is selected as a magnetic conductive layer of the electromagnetic shielding film, and a chemical expression of the iron-based amorphous alloy thin film of example 7 is Fe68Ni6.5Co3B13Si4C3Mo2.5. In the present embodiment, it is preferred that,the electromagnetic shielding film is sequentially provided with a protective layer, a magnetic conduction layer and a carrier layer, and the structure of the electromagnetic shielding film is shown in figure 1.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe68Ni6.5Co3B13Si4C3Mo2.5The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 18:
this example 18 provides an electromagnetic shielding film, where the iron-based amorphous alloy thin film of example 8 is selected as a magnetic conductive layer of the electromagnetic shielding film, and a chemical expression of the iron-based amorphous alloy thin film of example 8 is Fe62.8Ni12.7B11.8Si3.6S9.1. In this embodiment, the electromagnetic shielding film is sequentially arranged with a protective layer, a magnetic conductive layer and a carrier layer, and the structure thereof is as shown in fig. 1.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe62.8Ni12.7B11.8Si3.6S9.1The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 19:
this example 19 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film of example 10 is selected as a magnetic conductive layer of the electromagnetic shielding film, and a chemical expression of the iron-based amorphous alloy thin film of example 10 is Fe62.8Ni12.7B11.8Si3.6C9.1. In this embodiment, the electromagnetic shielding film is sequentially arranged with a protective layer, a magnetic conductive layer and a carrier layer, and the structure thereof is as shown in fig. 1.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe62.8Ni12.7B11.8Si3.6C9.1The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 20:
this example 20 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film of example 11 is selected as the magnetic conductive layer of the electromagnetic shielding film,the chemical expression of the Fe-based amorphous alloy thin film of example 11 is Fe62.8Ni12.7B11.8Si3.6P9.1. In this embodiment, the electromagnetic shielding film is sequentially arranged with a protective layer, a magnetic conductive layer and a carrier layer, and the structure thereof is as shown in fig. 1.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe62.8Ni12.7B11.8Si3.6P9.1The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 21:
this example 21 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film (chemical expression is Fe) of example 1 is selected as the magnetic conductive layer of the electromagnetic shielding film69Ni14B13Si4). In this embodiment, the electromagnetic shielding film is sequentially disposed with a protective layer, a conductive layer, a magnetic conductive layer, and a carrier layer, and the structure thereof is as shown in fig. 2.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe69Ni14B13Si4The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 22:
this example 22 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film (chemical expression is Fe) of example 1 is selected as the magnetic conductive layer of the electromagnetic shielding film69Ni14B13Si4). In this embodiment, the electromagnetic shielding film is sequentially disposed with a protective layer, a magnetic conduction layer, a conductive layer, a magnetic conduction layer, and a carrier layer, and the structure thereof is as shown in fig. 3.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe69Ni14B13Si4The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 23:
this example 23 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film of example 1 is selected as the magnetic conductive layer of the electromagnetic shielding filmThe chemical expression is Fe69Ni14B13Si4). In this embodiment, the electromagnetic shielding film is sequentially disposed with a protective layer, a magnetic conductive layer, a C fiber layer, a magnetic conductive layer, and a carrier layer, and the structure thereof is as shown in fig. 4.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe69Ni14B13Si4The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 24:
this example 24 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film (chemical expression is Fe) of example 1 is selected as the magnetic conductive layer of the electromagnetic shielding film69Ni14B13Si4). In this embodiment, the electromagnetic shielding film is sequentially arranged with a protective layer, a magnetic conductive layer and a carrier layer, and the structure thereof is as shown in fig. 1.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe62.8Ni12.7B11.8Si3.6C9.1The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 25:
this example 25 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film (chemical expression is Fe) of example 1 is selected as the magnetic conductive layer of the electromagnetic shielding film69Ni14B13Si4). In this embodiment, the electromagnetic shielding film is sequentially disposed with a protective layer, a conductive layer, a magnetic conductive layer, and a carrier layer, and the structure thereof is as shown in fig. 2.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe62.8Ni12.7B11.8Si3.6C9.1The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 26:
this example 26 provides an electromagnetic shielding film, wherein the iron-based amorphous alloy thin film (chemical expression is Fe) of example 1 is selected as the magnetic conductive layer of the electromagnetic shielding film69Ni14B13Si4). In this embodiment, the electromagnetic shielding film is sequentially disposed with a protective layer, a magnetic conduction layer, a conductive layer, a magnetic conduction layer, and a carrier layer, and the structure thereof is as shown in fig. 3.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe62.8Ni12.7B11.8Si3.6C9.1The protective layer is a polyester film, and the carrier layer is a polyimide film.
Example 27:
this example 27 provides an apparatus comprising an electromagnetic shielding film. The device provided by the embodiment can achieve a good electromagnetic shielding effect under high and low frequency electromagnetic fields.
Comparative example 1:
the comparative example 1 provides an electromagnetic shielding film, in which the chemical expression of the magnetic conductive layer of the electromagnetic shielding film is Fe6Co14B13Si4The iron-based amorphous alloy thin film is prepared by the preparation method of the iron-based amorphous alloy thin film, in the embodiment, the electromagnetic shielding film is sequentially provided with the protective layer, the magnetic conduction layer and the carrier layer, and the structure of the iron-based amorphous alloy thin film is shown in figure 1.
In this embodiment, the chemical expression of the magnetic conductive layer is Fe6Co14B13Si4The protective layer is a polyester film, and the carrier layer is a polyimide film.
Test example 1:
the electromagnetic shielding films of comparative example 1, examples 1, 12-17 were subjected to permeability test and electromagnetic shielding effectiveness test, and the test results are shown in table 1:
TABLE 1 permeability and shielding effectiveness of electromagnetic shielding film
The above test results show that the electromagnetic shielding films provided in examples 12 to 17 have higher magnetic permeability and shielding effectiveness at different electromagnetic frequencies, and the magnetic permeability and shielding effectiveness of examples 12 to 17 are higher than those of comparative example 1.
The iron-based amorphous alloy film provided by the invention is used as an electromagnetic shielding film made of a magnetic conduction layer, has high magnetic conductivity, can realize better shielding efficiency under different electromagnetic frequencies, has good magnetic shielding effect in a high-frequency electromagnetic field (more than 100kHz) and a low-frequency magnetic field (less than 100kHz), and has wider frequency application.
Test example 2:
the electromagnetic shielding films of example 2 and examples 14 to 16 were subjected to the shielding effectiveness test and the tensile strength test at different electromagnetic frequencies, and the test results are shown in table 2:
TABLE 2 Shielding effectiveness and tensile Strength of electromagnetic shielding film
The above test results show that the electromagnetic shielding films provided in examples 17 to 20 all have higher shielding effectiveness at different electromagnetic frequencies, and the tensile strengths of examples 18 to 20 are all higher than those of example 17 and comparative example 1 by more than 50%. This is because the C, P, S element with better flexibility is added in examples 18-20, and the C, P, S element is introduced into the fe-based amorphous alloy, so that the flexibility of the fe-based amorphous alloy can be effectively improved, and the fe-based amorphous alloy can be well applied to devices with higher requirements on flexibility, such as flexible circuit boards.
The application prospect of the electromagnetic shielding film is as follows:
in the electromagnetic shielding of modern power electronic products and equipment, the traditional material is difficult to have good electromagnetic shielding performance at a high frequency band and a low frequency band, generally has good shielding effect at the high frequency band, but has great shielding difficulty on low frequency and weak magnetic fields; or has better shielding effect in the middle and low frequency bands, but has higher shielding difficulty for high frequency and strong magnetic fields. The electromagnetic shielding material with the single-layer structure of the magnetic conduction layer, the double-layer structure of the magnetic conduction layer and the conducting layer and the multilayer composite structure of the magnetic conduction layer and the conducting layer is composed of an iron-based amorphous alloy film material with high magnetic conductivity and one or more of a metal shielding layer with high conductivity, a carbon nanotube shielding layer and a graphene shielding layer, and has excellent performances such as high magnetic conductivity, high saturation magnetic induction intensity and high conductivity. The high magnetic conductivity characteristic of the material can have a good shielding effect on low-frequency weak magnetic fields, and the high electric conductivity has a good shielding effect on electric fields and high-frequency magnetic fields. Therefore, the magnetic conduction layer single-layer structure, the magnetic conduction layer and conductive layer double-layer structure and the magnetic conduction layer and conductive layer multilayer composite structure covered by the invention effectively play the comprehensive advantages of electromagnetic shielding in high and low frequency electromagnetic fields, broaden the frequency spectrum bandwidth of the electromagnetic shielding and can meet the shielding performance of electromagnetic waves of various complex frequency bands. Therefore, the electromagnetic shielding film covered by the invention can have wide application prospect in electromagnetic shielding of various power electronic products and equipment (such as digital products like smart phones and watches, image display equipment, electric automobiles, measuring instruments, medical and military precision equipment and the like).
The above description is only a preferred embodiment of the present invention, and those skilled in the art may still modify the described embodiment without departing from the implementation principle of the present invention, and the corresponding modifications should also be regarded as the protection scope of the present invention.
Claims (20)
1. The iron-based amorphous alloy film is characterized by comprising the following components in percentage by mass: fe is more than or equal to 70 wt% and less than or equal to 90 wt%, Co is more than or equal to 0 wt% and less than or equal to 6 wt%, Si is more than or equal to 1 wt% and less than or equal to 4 wt%, B is more than or equal to 1 wt% and less than or equal to 3 wt%, Ni is more than 0.2 and less than or equal to 20 wt%, Mo is more than or equal to 0 and less than 6 wt%, and C is more than or equal to 0 and less than or equal to 3 wt%.
2. The Fe-based amorphous alloy thin film according to claim 1, wherein the composition further comprises any one or more of C, P, S elements, and the mass percentages of the elements are as follows: fe is more than or equal to 70 wt% and less than or equal to 90 wt%, Co is more than or equal to 0 wt% and less than or equal to 6 wt%, Si is more than or equal to 1 wt% and less than or equal to 4 wt%, B is more than or equal to 1 wt% and less than or equal to 3 wt%, Ni is more than or equal to 0.2 and less than or equal to 20 wt%, Mo is more than or equal to 0 and less than 6 wt%, C is more than or equal to 0 and less than or equal to 3 wt%, X is less than or equal to 0 and less than or equal to 5 wt%, and X is any one or more of C, P, S elements.
3. A method for preparing the fe-based amorphous alloy thin film according to claim 1, comprising the steps of:
s1, smelting the raw materials to obtain a master alloy, and finely processing the master alloy to obtain an iron-based alloy target; the raw materials comprise Fe, Co, B, Si, Ni, Mo and C, and the mass percentages of the elements are as follows: fe is more than or equal to 70 wt% and less than or equal to 90 wt%, Co is more than or equal to 0 wt% and less than or equal to 6 wt%, Si is more than or equal to 1 wt% and less than or equal to 4 wt%, B is more than or equal to 1 wt% and less than or equal to 3 wt%, Ni is more than 0.2 and less than or equal to 20 wt%, Mo is more than or equal to 0 and less than 6 wt%, C is more than or equal to 0 and less than or equal to 3 wt%;
s2, enabling the temperature of the substrate to be lower than 80 ℃, placing the substrate which is connected with the ground in parallel on the side surface of the iron-based alloy target, and keeping a distance L between the substrate and the iron-based alloy target, wherein the L is within a range of 2-10 cm; depositing on a substrate by adopting a magnetron sputtering method to obtain an amorphous iron-based amorphous alloy;
s3, keeping the power of the pulse power supply within the range of 2-10 kw, and depositing metal on the substrate for a time T to form the iron-based amorphous alloy film on the substrate.
4. The method of claim 3, wherein in step S1, the thickness of the Fe-based alloy target is 1-6 mm.
5. The method for preparing the Fe-based amorphous alloy thin film according to claim 3, wherein in the step S2 and the step S3, the deposition temperature of the substrate is less than 120 ℃ during magnetron sputtering; the working gas adopted by magnetron sputtering is Ar, and the vacuum degree after Ar is introduced is 1 multiplied by 10-1～5×10-1Pa; the working current of the magnetron sputtering is within the range of 4-12A, the linear speed of the coating film is 0.5-5 m/min, and the sputtering time T is 5-120 min.
6. The method of claim 5, wherein the working temperature of the working chamber is maintained at 25-100 ℃ during the coating in steps S2 and S3.
7. The method for preparing the Fe-based amorphous alloy film according to claim 3, wherein the thickness of the Fe-based amorphous alloy film is 20-2000 nm.
8. The method of claim 3, wherein in step S1, C, P, S elements are prepared as pure or mixed element targets, and the mass of the Fe-based alloy target and the pure or mixed element targets is 10: 1 to form a combined target material; in step S2, the temperature of the substrate is made to be less than 80 ℃, and the substrate connected to the ground is placed in parallel on the side surface of the combined target, and the distance L between the substrate and the combined target is kept, wherein L is in the range of 2-10 cm, and the amorphous iron-based amorphous alloy is obtained by depositing on the substrate by a magnetron sputtering method.
9. The method for preparing the Fe-based amorphous alloy film according to claim 8, wherein the thickness of the combined target material is 1-6 mm.
10. The method for preparing an Fe-based amorphous alloy thin film according to claim 8, wherein in the step S2 and the step S3, the deposition temperature of the substrate is less than 120 ℃ during magnetron sputtering; the working gas adopted by magnetron sputtering is Ar, and the vacuum degree after Ar is introduced is 1 multiplied by 10-1～5×10-1Pa; the working current of the magnetron sputtering is within the range of 4-12A, the linear speed of the coating film is 0.5-5 m/min, and the sputtering time T is 5-120 min.
11. The method of claim 10, wherein the working temperature of the working chamber is maintained at 25-100 ℃ during the coating in steps S2 and S3.
12. The method for preparing the Fe-based amorphous alloy film according to claim 8, wherein the thickness of the Fe-based amorphous alloy film is 20-2000 nm.
13. An electromagnetic shielding film using the iron-based amorphous alloy thin film as claimed in any one of claims 1 to 2, comprising a carrier layer, a magnetic conduction layer and a protective layer, which are sequentially arranged, wherein the magnetic conduction layer is the iron-based amorphous alloy thin film.
14. The electromagnetic shielding film according to claim 13, wherein the magnetic conductive layer is formed by sequentially arranging a plurality of iron-based amorphous alloy thin films.
15. The electromagnetic shielding film of the fe-based amorphous alloy thin film according to claim 14, wherein any one or more of a C-fiber layer, a P-fiber layer, and an S-fiber layer are disposed between adjacent magnetic conductive layers.
16. The electromagnetic shielding film according to claim 13, wherein a conductive layer is disposed between the magnetic conductive layer and the protective layer, and the conductive layer is one of a metal shielding layer, a carbon nanotube shielding layer, and a graphene shielding layer or is formed by sequentially disposing any of a metal shielding layer, a carbon nanotube shielding layer, and a graphene shielding layer.
17. The electromagnetic shielding film according to claim 16, wherein the metallic shielding layer comprises a single metallic shielding layer and/or an alloy shielding layer; the single metal shielding layer is made of any one of aluminum, titanium, zinc, iron, nickel, chromium, cobalt, copper, silver and gold, and the alloy shielding layer is made of any two or more of aluminum, titanium, zinc, iron, nickel, chromium, cobalt, copper, silver and gold.
18. The electromagnetic shielding film of claim 16, wherein adjacent conductive layers and magnetic conductive layers are connected by one or more of electroless plating, PVD, CVD, evaporation plating, sputter plating, electroplating, or composite plating.
19. The electromagnetic shielding film according to claim 13, wherein the protective layer and the carrier layer are any one of a PPS film layer, a PEN film layer, a polyester film layer, a polyimide film layer, a film layer formed after curing epoxy resin ink, a film layer formed after curing urethane ink, a film layer formed after curing modified acrylic resin, and a film layer formed after curing polyimide resin.
20. An apparatus comprising the electro-magnetic shielding film of any one of claims 13-19.
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| CN105671461A (en) * | 2016-04-05 | 2016-06-15 | 广州齐达材料科技有限公司 | Non-crystalline material, and preparation method and application thereof |
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| CN207151084U (en) * | 2017-04-05 | 2018-03-27 | 合肥美凯电子有限公司 | A kind of novel electromagnetic shielding film |
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| CN109207871A (en) * | 2018-09-19 | 2019-01-15 | 安徽工业大学 | A kind of amorphous-nano-crystalline magnetically soft alloy and preparation method thereof |
| CN113286913A (en) * | 2019-01-09 | 2021-08-20 | 王静然 | Amorphous strip master alloy and preparation method thereof |
| CN109778082A (en) * | 2019-01-24 | 2019-05-21 | 南京航空航天大学 | A kind of Fe-based amorphous alloy and its preparation method and application of high/low temperature annealing toughness |
| US20200324373A1 (en) * | 2019-04-15 | 2020-10-15 | Baolong Shen | Iron-based amorphous nanocrystalline laser cladding composite coating, preparation method and test method thereof |
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