CN110777342A - Magnetostrictive film and preparation method thereof - Google Patents

Magnetostrictive film and preparation method thereof Download PDF

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Publication number
CN110777342A
CN110777342A CN201911004945.XA CN201911004945A CN110777342A CN 110777342 A CN110777342 A CN 110777342A CN 201911004945 A CN201911004945 A CN 201911004945A CN 110777342 A CN110777342 A CN 110777342A
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China
Prior art keywords
target
film
sputtered
fega
power supply
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CN201911004945.XA
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朱婧
门阔
连紫薇
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GRIMN Engineering Technology Research Institute Co Ltd
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GRIMN Engineering Technology Research Institute Co Ltd
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Priority to CN201911004945.XA priority Critical patent/CN110777342A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/16Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/14Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
    • H01F41/18Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering

Abstract

The invention discloses a magnetostrictive film and a preparation method thereof, wherein the film is a FeGaB amorphous film deposited on a single-side polished monocrystalline silicon substrate, and the thickness of the film is 400-800 nm; the preparation method comprises the following steps: cleaning a single-side polished single crystal silicon substrate; and depositing the FeGaB film on the substrate by co-sputtering by adopting a magnetron sputtering method. The magnetostrictive film prepared by the method has the advantages of good soft magnetic performance, low saturation field, high magnetostrictive coefficient and the like. The invention can be used for preparing the magnetoelectric composite film with miniaturization, high magnetoelectric coupling coefficient under the megahertz condition and excellent comprehensive performance.

Description

Magnetostrictive film and preparation method thereof
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a magnetostrictive film and a preparation method thereof.
Background
The magnetoelectric composite material is valued by researchers because of the advantages of high Curie temperature, high sensitivity, excellent magneto-electromechanical coupling performance, simple structure, low cost and the like. Among other things, the magnetic material layer should have characteristics of high saturation magnetostriction constant and low saturation field. At present, a high-quality metal soft magnetic film can be deposited at room temperature by a physical vapor deposition method, and the metal soft magnetic film is low in cost and easy to integrate into different integrated circuits. However, a metal magnetic thin film having a large saturation magnetostriction constant and a low saturation field is not easily obtained. In the selection of the magnetostrictive layer, Terfenol-D (TbDyFe with a Laves phase structure) has a large magnetostrictive coefficient, but the Terfenol-D-based magnetoelectric composite material is not suitable for application in a low field due to relatively low magnetic permeability and high saturation magnetic field; the amorphous FeBSiC alloy has the magnetic conductivity as high as 40000, but the magnetostriction coefficient is relatively small; compared with two materials of FeBSiC and Terfenol-D, the FeGaB material has the advantages of the FeBSiC and the Terfenol-D, and the FeGaB film has better low magnetic field response performance than the Terfenol-D film and has a larger magnetostriction coefficient than the FeBSiC film. More importantly, the matching degree of the two materials of FeGaB/AlN is higher. However, when the content of B is different, the film formation is significantly affected, and therefore, the composition of the film needs to be optimized.
Disclosure of Invention
The invention aims to provide a magnetostrictive film which has the advantages of good soft magnetic performance, low saturation field and high magnetostrictive coefficient.
The invention also aims to provide a preparation method of the magnetostrictive film, which can be used for preparing a magnetoelectric composite film with miniaturization, high magnetoelectric coupling coefficient under the megahertz condition and excellent comprehensive performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a magnetostrictive film comprises the following steps:
(1) cleaning single-side polished monocrystalline silicon, and putting the single-side polished monocrystalline silicon on a substrate table of ultrahigh vacuum magnetron sputtering equipment to prepare film coating;
(2) placing a FeGa target and a B target to be sputtered on a target seat;
(3) when the silicon chip is sputtered and deposited, the FeGa target is sputtered by a direct current power supply, the B target is sputtered by a radio frequency power supply, and the FeGa target and the radio frequency power supply are co-sputtered to reach the required thickness.
Further, in the step (1), the single-side polished monocrystalline silicon is respectively ultrasonically cleaned for 15-30 minutes by alcohol and acetone, and then dried by electric air blowing.
Further, in the step (3), the sputtering deposition is performed in an inert atmosphere.
Further, in the step (3), the power of the direct current power supply selected by the FeGa target is 60W, the power of the radio frequency power supply selected by the B target is 60W, the deposition rate of the film is 13nm per minute, and the sputtering time is 30-60 min. The working pressure is 1 Pa.
The magnetostrictive film prepared by the method is a FeGaB amorphous film deposited on a single-side polished monocrystalline silicon substrate, and the FeGaB film is formed by co-sputtering a FeGa target and a B target and has the thickness of 400-800 nm.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts magnetron sputtering technology, and the FeGaB film is deposited on the monocrystalline silicon substrate, so that the invention has the advantages of good soft magnetic performance, low saturation field, high magnetostriction coefficient and the like. The method has the advantages of simple operation, low cost and easy industrial realization and popularization.
Drawings
FIG. 1 is a VSM curve of a 400nm thick film prepared according to the present invention.
FIG. 2 is a VSM curve of a 800nm thick film prepared according to the present invention.
Detailed Description
The present invention is further described in detail below with reference to the drawings and examples, but the scope of the present invention is not limited thereto.
Example 1
The preparation process of the magnetostrictive film in this example is as follows:
1) cutting the single-side polished monocrystalline silicon wafer into the size of an objective table by using a diamond blade, respectively ultrasonically cleaning the monocrystalline silicon wafer for 15min by using absolute ethyl alcohol and acetone, blow-drying the monocrystalline silicon wafer by using an electric hair drier, and putting the monocrystalline silicon wafer on a substrate table of ultrahigh vacuum magnetron sputtering equipment.
2) The target material is arranged on the target material seat, the iron gallium target material is connected with a direct current power supply, and the boron target material is connected with a radio frequency power supply. After the target material is arranged, the sputtering cabin door is closed, the cooling machine is started, the mechanical pump is firstly used for pre-vacuumizing, and when the vacuum degree reaches 10 -1mba turn on the molecular pump.
3) When in useThe background vacuum degree reaches 5.4 multiplied by 10 -7mba, opening a gas cylinder valve, adjusting the flow, adjusting the substrate temperature, turning on a power supply, adjusting the power and sputtering.
4) Deposition process parameters of the FeGaB film are as follows: the protective gas is argon, the working pressure is 1Pa, the gas flow is 20sccm, the power of a direct current power supply is 60W, the power of a radio frequency power supply is 60W, and the additional substrate table rotates. Under this parameter, the deposition rate was about 13nm per minute, which was accurately obtained before plating. And depositing for 30 min. The power is turned off.
5) The film component is Fe after testing 76Ga 8B 16And the thickness is 400 nm.
6) Fig. 1 is a VSM curve of a thin film. Therefore, the FeGaB film plated under the parameters of the embodiment has good soft magnetic performance and low saturation magnetic field.
7) The magnetostriction coefficient of the film can reach 130ppm through testing.
Example 2
The preparation process of the magnetostrictive film in this example is as follows:
1) cutting the single-side polished monocrystalline silicon wafer into the size of an objective table by using a diamond blade, respectively ultrasonically cleaning the monocrystalline silicon wafer for 15min by using absolute ethyl alcohol and acetone, blow-drying the monocrystalline silicon wafer by using an electric hair drier, and putting the monocrystalline silicon wafer on a substrate table of ultrahigh vacuum magnetron sputtering equipment.
2) The target material is arranged on the target material seat, the iron gallium target material is connected with a direct current power supply, and the boron target material is connected with a radio frequency power supply. After the target material is arranged, the sputtering cabin door is closed, the cooling machine is started, the mechanical pump is firstly used for pre-vacuumizing, and when the vacuum degree reaches 10 -1mba turn on the molecular pump.
3) When the background vacuum degree reaches 5.4 multiplied by 10 -7mba, opening a gas cylinder valve, adjusting the flow, adjusting the substrate temperature, turning on a power supply, adjusting the power and sputtering.
4) Deposition process parameters of the FeGaB film are as follows: the protective gas is argon, the working pressure is 1Pa, the gas flow is 20sccm, the power of a direct current power supply is 60W, the power of a radio frequency power supply is 60W, and the additional substrate table rotates. Under this parameter, the deposition rate was about 13nm per minute, which was accurately obtained before plating. And depositing for 60 min. The power is turned off.
5) The film component is Fe after testing 76Ga 8B 16The thickness is 800 nm.
6) Fig. 2 is a VSM curve of a thin film. Therefore, the FeGaB film plated under the parameters of the embodiment has good soft magnetic performance and low saturation magnetic field.
7) The magnetostriction coefficient of the film can reach 160ppm through testing.
The above embodiments describe the technical solutions of the present invention in detail. It will be clear that the invention is not limited to the described embodiments. Based on the embodiments of the present invention, those skilled in the art can make various changes, but any changes equivalent or similar to the present invention are within the protection scope of the present invention.

Claims (6)

1. A preparation method of a magnetostrictive film is characterized by comprising the following steps:
(1) cleaning single-side polished monocrystalline silicon, and putting the single-side polished monocrystalline silicon on a substrate table of ultrahigh vacuum magnetron sputtering equipment to prepare film coating;
(2) placing a FeGa target and a B target to be sputtered on a target seat;
(3) and carrying out silicon wafer sputtering deposition to enable the FeGa target and the B target to be co-sputtered to reach the required thickness.
2. The method according to claim 1, wherein in the step (1), the cleaning of the single-side polished single-crystal silicon is performed by ultrasonic cleaning with alcohol and acetone for 15 to 30 minutes, respectively, and then blow-drying with electric blow.
3. The method according to claim 1, wherein in the step (3), the FeGa target is sputtered by using a direct current power supply, and the B target is sputtered by using a radio frequency power supply.
4. The method of claim 1, wherein in step (3), the sputter depositing is performed in an inert atmosphere.
5. The method according to claim 1, wherein in the step (3), the FeGa target is sputtered with a DC power supply power of 60W, the B target is sputtered with a RF power supply power of 60W, the film deposition rate is 13nm per minute, and the sputtering time is 30-60 min; the working pressure is 1 Pa.
6. The magnetostrictive film prepared by the method according to any one of claims 1-5, wherein the film is a FeGaB amorphous film formed by co-sputtering a FeGa target and a B target and has a thickness of 400-800 nm.
CN201911004945.XA 2019-10-22 2019-10-22 Magnetostrictive film and preparation method thereof Pending CN110777342A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114774858A (en) * 2022-03-29 2022-07-22 福建师范大学 Tunable ferromagnetic resonance composite film and preparation method thereof
CN115612988A (en) * 2022-10-18 2023-01-17 西南应用磁学研究所(中国电子科技集团公司第九研究所) High-magnetic-performance FeGaB magnetoelectric film and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0373615A2 (en) * 1988-12-15 1990-06-20 Matsushita Electric Industrial Co., Ltd. Soft magnetic alloy films and the method of manufacturing the same
CN110212085A (en) * 2019-06-03 2019-09-06 西安交通大学 Adjustable giant magnetoresistance sensor of measurement range and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0373615A2 (en) * 1988-12-15 1990-06-20 Matsushita Electric Industrial Co., Ltd. Soft magnetic alloy films and the method of manufacturing the same
CN110212085A (en) * 2019-06-03 2019-09-06 西安交通大学 Adjustable giant magnetoresistance sensor of measurement range and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
尹冠博: "AlN/FeGaB磁电复合材料的制备与性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114774858A (en) * 2022-03-29 2022-07-22 福建师范大学 Tunable ferromagnetic resonance composite film and preparation method thereof
CN115612988A (en) * 2022-10-18 2023-01-17 西南应用磁学研究所(中国电子科技集团公司第九研究所) High-magnetic-performance FeGaB magnetoelectric film and preparation method thereof

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