CN108950505B - CaB with strong ferromagnetism6Method for producing thin film - Google Patents

CaB with strong ferromagnetism6Method for producing thin film Download PDF

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CN108950505B
CN108950505B CN201810888661.0A CN201810888661A CN108950505B CN 108950505 B CN108950505 B CN 108950505B CN 201810888661 A CN201810888661 A CN 201810888661A CN 108950505 B CN108950505 B CN 108950505B
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CN108950505A (en
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康丽纳
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GUANGDONG GUANHAO HIGH-TECH CO LTD
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Quanzhou Kangxin Chemical Technology Co ltd
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/361—Coatings of the type glass/metal/inorganic compound/metal/inorganic compound/other
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • 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
    • C23C14/067—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
    • 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
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • 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
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering

Abstract

The invention discloses a preparation method of a CaB6 film with strong ferromagnetism, which comprises the following steps: preparing a glass substrate; depositing a CuGe layer on a glass substrate by taking a CuGe alloy as a target, wherein the thickness of the CuGe layer is 15-30 nm; depositing a CoPbMnO layer on the CuGe layer by taking the CoPbMn alloy as a target, wherein the thickness of the CoPbMnO layer is 20-40 nm; depositing a DyZn layer on the CoPbMnO layer by taking DyZn alloy as a target material, wherein the thickness of the DyZn layer is 10-30 nm; depositing a first NdFeB layer on the DyZn layer by taking the NdFeB as a target material, wherein the thickness of the first NdFeB layer is 20-40 nm; depositing a PrZn layer on the first NdFeB layer by taking the PrZn alloy as a target material, wherein the thickness of the PrZn layer is 5-10 nm; depositing a second NdFeB layer on the PrZn layer by taking the NdFeB as a target material, wherein the thickness of the second NdFeB layer is 10-20 nm; and depositing a CaB6 layer on the second NdFeB layer by taking CaB6 as a target, wherein the thickness of the CaB6 layer is 30-50 nm. The preparation method of the invention improves the saturation magnetization of the whole material.

Description

Preparation method of CaB6 film with strong ferromagnetism
Technical Field
The invention relates to the field of information functional materials, in particular to a preparation method of a CaB6 film with strong ferromagnetism.
Background
Boride has the properties of high hardness, high melting point and the like, has stable chemical properties, can be used for refractory materials, grinding materials, superconducting materials and the like, and has an important position in modern industry. Calcium hexaboride (CAB6) has the common characteristics of boride, and also has the excellent characteristics of constant specific resistance, zero thermal expansion value within a certain range, high neutron absorption coefficient, low electron work function and the like, and is often used as an antioxidant and a deoxidizer in industrial copper alloy production, a neutron absorption and protection material in nuclear industry and the like. Since d.p.young found weak ferromagnetism at high temperature in La-doped CaB6, many researchers investigated the cause of this phenomenon through sample experiments or theoretical simulations. Since ferromagnetism is very sensitive to lattice constant and crystal structure, it was also found in studies that europium (Eu), gadolinium (Gd), and thorium doped CaB6 is also ferromagnetic. The ferromagnetic elements are generally transition metal elements with unfilled 3d, 4f or 5f shells, while the CaB6 does not contain magnetic transition metal impurities, and the resulting magnetic properties are referred to as d0 ferromagnetism. Since the abnormal ferromagnetism such as CaB6 cannot be explained by the conventional electronic theory, it has attracted more and more people to conduct related research. The CaB6 thin film becomes a new material with ferromagnetism, and the CaB6 thin film material is expected to become a novel soft magnetic material due to the higher resistivity of the CaB6
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide a preparation method of a CaB6 thin film with strong ferromagnetism, which can overcome the defects of the prior art.
In order to achieve the above object, the present invention provides a method for preparing a CaB6 thin film with strong ferromagnetic properties, comprising the following steps: preparing a glass substrate; depositing a CuGe layer on a glass substrate by taking a CuGe alloy as a target, wherein the thickness of the CuGe layer is 15-30 nm; depositing a CoPbMnO layer on the CuGe layer by taking the CoPbMn alloy as a target, wherein the thickness of the CoPbMnO layer is 20-40 nm; depositing a DyZn layer on the CoPbMnO layer by taking DyZn alloy as a target material, wherein the thickness of the DyZn layer is 10-30 nm; depositing a first NdFeB layer on the DyZn layer by taking the NdFeB as a target material, wherein the thickness of the first NdFeB layer is 20-40 nm; depositing a PrZn layer on the first NdFeB layer by taking the PrZn alloy as a target material, wherein the thickness of the PrZn layer is 5-10 nm; depositing a second NdFeB layer on the PrZn layer by taking the NdFeB as a target material, wherein the thickness of the second NdFeB layer is 10-20 nm; and depositing a CaB6 layer on the second NdFeB layer by taking CaB6 as a target, wherein the thickness of the CaB6 layer is 30-50 nm.
In a preferred embodiment, the nominal chemical formula of the CuGe alloy is Cu100-xGexX is 8-10, and wherein depositing the CuGe layer on the glass substrate is performed under the following conditions: the radio frequency magnetron sputtering method is adopted, the sputtering atmosphere is argon, the sputtering pressure is 2-3Pa, the sputtering power is 100-150W, the sputtering voltage is 300-500V, and the substrate temperature is 300-400 ℃.
In a preferred embodiment, the CoPbMn alloy target has a nominal chemical formula of CoaPbbMn100-a-bA-3-6, b-20-40, and wherein the deposition of the CoPbMnO layer on the CuGe layer is under the following conditionsThe following steps are carried out: the reactive radio frequency magnetron sputtering method is adopted, the sputtering atmosphere is oxygen, the sputtering pressure is 5-6Pa, the sputtering power is 500W-.
In a preferred embodiment, the deposition of the DyZn layer on the CoPbMnO layer is performed under the following conditions: the radio frequency magnetron sputtering method is adopted, the sputtering atmosphere is argon, the sputtering pressure is 3-5Pa, the sputtering power is 150-200W, the sputtering voltage is 200-300V, and the substrate temperature is 400-500 ℃.
In a preferred embodiment, the deposition of the first NdFeB layer on the DyZn layer is carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3-5Pa, the sputtering power is 150-250W, the sputtering voltage is 200-300V, and the substrate temperature is 150-300 ℃.
In a preferred embodiment, the deposition of the PrZn layer on the first NdFeB layer is carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3-5Pa, the sputtering power is 50-100W, the sputtering voltage is 150-200V, and the substrate temperature is 250-350 ℃.
In a preferred embodiment, the deposition of the second NdFeB layer on the PrZn layer is carried out under the following conditions: the radio frequency magnetron sputtering method is adopted, the sputtering atmosphere is argon, the sputtering pressure is 3-5Pa, the sputtering power is 150-250W, the sputtering voltage is 200-300V, and the substrate temperature is 500-600 ℃.
In a preferred embodiment, the deposition of the CaB6 layer on the second NdFeB layer is carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3-5Pa, the sputtering power is 100-150W, the sputtering voltage is 100-150V, and the substrate temperature is 250-350 ℃.
Compared with the prior art, the invention has the following advantages: the CaB6 thin film is a new material with ferromagnetism, and the CaB6 has high resistivity, so the CaB6 thin film material is expected to be a novel soft magnetic material. The difficulty encountered in the research of the CaB6 film material at present is that: it is difficult to further increase the saturation magnetization of CaB6 thin film by conventional methods (doping, changing the manufacturing process, heat treatment), and a smaller saturation magnetization means that the size of the thin film material must be increased in order to achieve a signal strength of a considerable size, i.e. the device must be made larger to meet the requirements of magnetic recording. In order to overcome the defects of the prior art, the invention provides a brand-new method for increasing the saturation magnetization of a CaB6 thin film and reducing the coercive force of a CaB6 material, and the method of the invention increases the saturation magnetization exhibited by a CaB6 layer through magnetic coupling by means of increasing the number of film layers and plating other magnetic layers below the CaB6 layer. The structure of the invention not only keeps the high resistivity of CaB6 (because CaB6 is positioned on the surface of the material), but also improves the saturation magnetization of the whole material and obtains good technical effect.
Drawings
FIG. 1 is a flow chart of a method of making according to an embodiment of the present invention.
Fig. 2 is a schematic diagram of a product structure according to an embodiment of the invention.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
FIG. 1 is a flow chart of a method of making according to an embodiment of the present invention. Fig. 2 is a schematic diagram of a product structure according to an embodiment of the invention. As shown in the figure, the preparation method comprises the following steps:
step 101: preparing a glass substrate 201;
step 102: depositing a CuGe layer 202 on a glass substrate by taking a CuGe alloy as a target, wherein the thickness of the CuGe layer is 15-30 nm;
step 103: depositing a CoPbMnO layer 203 on the CuGe layer by taking the CoPbMn alloy as a target material, wherein the thickness of the CoPbMnO layer is 20-40 nm;
step 104: depositing a DyZn layer 204 on the CoPbMnO layer by taking DyZn alloy as a target (wherein the atomic ratio of Dy to Zn in the DyZn alloy is 1:1), wherein the thickness of the DyZn layer is 10-30 nm;
step 105: depositing a first NdFeB layer 205 on the DyZn layer using NdFeB as a target (the NdFeB target has the composition of a common NdFeB permanent magnetic material), wherein the thickness of the first NdFeB layer is 20-40 nm;
step 106: depositing a PrZn layer 206 on the first NdFeB layer by taking a PrZn alloy as a target (wherein the atomic ratio of Pr to Zn in the PrZn alloy is 1:1), wherein the thickness of the PrZn layer is 5-10 nm;
step 107: depositing a second NdFeB layer 207 on the PrZn layer by taking the NdFeB as a target material, wherein the thickness of the second NdFeB layer is 10-20 nm; and
step 108: and depositing a CaB6 layer 208 on the second NdFeB layer by taking CaB6 as a target, wherein the thickness of the CaB6 layer is 30-50 nm.
Example 1
The preparation method of the CaB6 film with strong ferromagnetism comprises the following steps: preparing a glass substrate; depositing a CuGe layer on a glass substrate by using a CuGe alloy as a target, wherein the thickness of the CuGe layer is 15 nm; depositing a CoPbMnO layer on the CuGe layer by taking the CoPbMn alloy as a target, wherein the thickness of the CoPbMnO layer is 20 nm; depositing a DyZn layer on the CoPbMnO layer by taking DyZn alloy as a target material, wherein the thickness of the DyZn layer is 10 nm; depositing a first NdFeB layer on the DyZn layer by taking the NdFeB as a target material, wherein the thickness of the first NdFeB layer is 20 nm; depositing a PrZn layer on the first NdFeB layer by taking the PrZn alloy as a target material, wherein the thickness of the PrZn layer is 5 nm; depositing a second NdFeB layer on the PrZn layer by taking the NdFeB as a target material, wherein the thickness of the second NdFeB layer is 10 nm; and depositing a CaB6 layer on the second NdFeB layer by taking CaB6 as a target, wherein the thickness of the CaB6 layer is 30 nm. Wherein the nominal chemical formula of the CuGe alloy is Cu100-xGexAnd x is 8, and wherein depositing the CuGe layer on the glass substrate is performed under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 2Pa, the sputtering power is 100W, the sputtering voltage is 300V, and the substrate temperature is 300 ℃. Wherein the nominal chemical formula of the CoPbMn alloy target material is CoaPbbMn100-a-bAnd a is 3 and b is 20, and wherein the deposition of the CoPbMnO layer on the CuGe layer is performed under the following conditions: adopting a reactive radio frequency magnetron sputtering method, wherein the sputtering atmosphere is oxygen, the sputtering pressure is 5Pa, the sputtering power is 300W, the sputtering voltage is 400V, and the substrate temperature is 300 ℃. The deposition of the DyZn layer on the CoPbMnO layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3Pa, the sputtering power is 150W, the sputtering voltage is 200V, and the substrate temperature is 400 ℃. The deposition of the first NdFeB layer on the DyZn layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3Pa, the sputtering power is 150W, the sputtering voltage is 200V, and the substrate temperature is 150 ℃. The deposition of the PrZn layer on the first NdFeB layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3Pa, the sputtering power is 50W, the sputtering voltage is 150V, and the substrate temperature is 250 ℃. The deposition of the second NdFeB layer on the PrZn layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3Pa, the sputtering power is 150W, the sputtering voltage is 200V, and the substrate temperature is 500 ℃. The deposition of the CaB6 layer on the second NdFeB layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3Pa, the sputtering power is 100W, the sputtering voltage is 100V, and the substrate temperature is 250 ℃.
Example 2
The preparation method of the CaB6 film with strong ferromagnetism comprises the following steps: preparing a glass substrate; depositing a CuGe layer on a glass substrate by using a CuGe alloy as a target, wherein the thickness of the CuGe layer is 30 nm; depositing a CoPbMnO layer on the CuGe layer by taking the CoPbMn alloy as a target, wherein the thickness of the CoPbMnO layer is 40 nm; depositing a DyZn layer on the CoPbMnO layer by taking DyZn alloy as a target material, wherein the thickness of the DyZn layer is 30 nm; depositing a first NdFeB layer on the DyZn layer by taking the NdFeB as a target material, wherein the thickness of the first NdFeB layer is 40 nm; depositing a PrZn layer on the first NdFeB layer by taking the PrZn alloy as a target material, wherein the thickness of the PrZn layer is 10 nm; depositing a second NdFeB layer on the PrZn layer by taking the NdFeB as a target material, wherein the thickness of the second NdFeB layer is 20 nm; CaB6 as target material in the second NdFeBAnd depositing a CaB6 layer on the layer, wherein the thickness of the CaB6 layer is 50 nm. Wherein the nominal chemical formula of the CuGe alloy is Cu100-xGexX is 10, and wherein depositing the CuGe layer on the glass substrate is performed under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3Pa, the sputtering power is 150W, the sputtering voltage is 500V, and the substrate temperature is 400 ℃. Wherein the nominal chemical formula of the CoPbMn alloy target material is CoaPbbMn100-a-bWhere a is 6 and b is 40, and where the deposition of the CoPbMnO layer on the CuGe layer is performed under the following conditions: by adopting a reactive radio frequency magnetron sputtering method, the sputtering atmosphere is oxygen, the sputtering pressure is 6Pa, the sputtering power is 500W, the sputtering voltage is 600V, and the substrate temperature is 400 ℃. The deposition of the DyZn layer on the CoPbMnO layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 5Pa, the sputtering power is 200W, the sputtering voltage is 300V, and the substrate temperature is 500 ℃. The deposition of the first NdFeB layer on the DyZn layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 5Pa, the sputtering power is 250W, the sputtering voltage is 300V, and the substrate temperature is 300 ℃. The deposition of the PrZn layer on the first NdFeB layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 5Pa, the sputtering power is 100W, the sputtering voltage is 200V, and the substrate temperature is 350 ℃. The deposition of the second NdFeB layer on the PrZn layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 5Pa, the sputtering power is 250W, the sputtering voltage is 300V, and the substrate temperature is 600 ℃. The deposition of the CaB6 layer on the second NdFeB layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 5Pa, the sputtering power is 150W, the sputtering voltage is 150V, and the substrate temperature is 350 ℃.
Example 3
The preparation method of the CaB6 film with strong ferromagnetism comprises the following steps: preparing a glass substrate; depositing a CuGe layer on a glass substrate by using a CuGe alloy as a target, wherein the thickness of the CuGe layer is 20 nm; using CoPbMn alloy as a target material, and depositing a CoPbMnO layer on the CuGe layer, whereinThe thickness of the CoPbMnO layer is 25 nm; depositing a DyZn layer on the CoPbMnO layer by taking DyZn alloy as a target material, wherein the thickness of the DyZn layer is 15 nm; depositing a first NdFeB layer on the DyZn layer by taking the NdFeB as a target, wherein the thickness of the first NdFeB layer is 25 nm; depositing a PrZn layer on the first NdFeB layer by taking the PrZn alloy as a target material, wherein the thickness of the PrZn layer is 6 nm; depositing a second NdFeB layer on the PrZn layer by taking the NdFeB as a target material, wherein the thickness of the second NdFeB layer is 15 nm; and depositing a CaB6 layer on the second NdFeB layer by taking CaB6 as a target, wherein the thickness of the CaB6 layer is 35 nm. Wherein the nominal chemical formula of the CuGe alloy is Cu100-xGexX is 8.5, and wherein depositing the CuGe layer on the glass substrate is performed under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 2.5Pa, the sputtering power is 110W, the sputtering voltage is 320V, and the substrate temperature is 320 ℃. Wherein the nominal chemical formula of the CoPbMn alloy target material is CoaPbbMn100-a-bAnd a-4 and b-25, and wherein depositing the CoPbMnO layer on the CuGe layer is performed under the following conditions: the method adopts a reactive radio frequency magnetron sputtering method, the sputtering atmosphere is oxygen, the sputtering pressure is 5.5Pa, the sputtering power is 350W, the sputtering voltage is 450V, and the substrate temperature is 320 ℃. The deposition of the DyZn layer on the CoPbMnO layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3.5Pa, the sputtering power is 160W, the sputtering voltage is 220V, and the substrate temperature is 420 ℃. The deposition of the first NdFeB layer on the DyZn layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3.5Pa, the sputtering power is 180W, the sputtering voltage is 220V, and the substrate temperature is 180 ℃. The deposition of the PrZn layer on the first NdFeB layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3.5Pa, the sputtering power is 60W, the sputtering voltage is 160V, and the substrate temperature is 260 ℃. The deposition of the second NdFeB layer on the PrZn layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3.5Pa, the sputtering power is 180W, the sputtering voltage is 220V, and the substrate temperature is 520 ℃. The deposition of the CaB6 layer on the second NdFeB layer was carried out under the following conditions: by radio frequency magnetron sputteringThe method comprises the steps of adopting argon as sputtering atmosphere, adopting sputtering pressure of 3.5Pa, adopting sputtering power of 110W, adopting sputtering voltage of 110V and adopting substrate temperature of 280 ℃.
Example 4
The preparation method of the CaB6 film with strong ferromagnetism comprises the following steps: preparing a glass substrate; depositing a CuGe layer on a glass substrate by using a CuGe alloy as a target, wherein the thickness of the CuGe layer is 25 nm; depositing a CoPbMnO layer on the CuGe layer by taking the CoPbMn alloy as a target, wherein the thickness of the CoPbMnO layer is 30 nm; depositing a DyZn layer on the CoPbMnO layer by taking DyZn alloy as a target material, wherein the thickness of the DyZn layer is 20 nm; depositing a first NdFeB layer on the DyZn layer by taking the NdFeB as a target material, wherein the thickness of the first NdFeB layer is 30 nm; depositing a PrZn layer on the first NdFeB layer by taking the PrZn alloy as a target material, wherein the thickness of the PrZn layer is 7 nm; depositing a second NdFeB layer on the PrZn layer by taking the NdFeB as a target material, wherein the thickness of the second NdFeB layer is 15 nm; and depositing a CaB6 layer on the second NdFeB layer by taking CaB6 as a target, wherein the thickness of the CaB6 layer is 40 nm. Wherein the nominal chemical formula of the CuGe alloy is Cu100-xGexAnd x is 9, and wherein depositing the CuGe layer on the glass substrate is performed under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 2.5Pa, the sputtering power is 120W, the sputtering voltage is 400V, and the substrate temperature is 350 ℃. Wherein the nominal chemical formula of the CoPbMn alloy target material is CoaPbbMn100-a-bAnd a-5 and b-30, and wherein depositing the CoPbMnO layer on the CuGe layer is performed under the following conditions: the method adopts a reactive radio frequency magnetron sputtering method, the sputtering atmosphere is oxygen, the sputtering pressure is 5.5Pa, the sputtering power is 400W, the sputtering voltage is 500V, and the substrate temperature is 350 ℃. The deposition of the DyZn layer on the CoPbMnO layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 4Pa, the sputtering power is 180W, the sputtering voltage is 250V, and the substrate temperature is 450 ℃. The deposition of the first NdFeB layer on the DyZn layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 4Pa, the sputtering power is 200W, the sputtering voltage is 250V, and the substrate temperature is 200 ℃. The deposition of the PrZn layer on the first NdFeB layer was carried out under the following conditions:adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 4Pa, the sputtering power is 80W, the sputtering voltage is 180V, and the substrate temperature is 300 ℃. The deposition of the second NdFeB layer on the PrZn layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 4Pa, the sputtering power is 200W, the sputtering voltage is 250V, and the substrate temperature is 550 ℃. The deposition of the CaB6 layer on the second NdFeB layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 4Pa, the sputtering power is 120W, the sputtering voltage is 120V, and the substrate temperature is 300 ℃.
Example 5
The preparation method of the CaB6 film with strong ferromagnetism comprises the following steps: preparing a glass substrate; depositing a CuGe layer on a glass substrate by using a CuGe alloy as a target, wherein the thickness of the CuGe layer is 25 nm; depositing a CoPbMnO layer on the CuGe layer by taking the CoPbMn alloy as a target, wherein the thickness of the CoPbMnO layer is 35 nm; depositing a DyZn layer on the CoPbMnO layer by taking DyZn alloy as a target, wherein the thickness of the DyZn layer is 25 nm; depositing a first NdFeB layer on the DyZn layer by taking the NdFeB as a target material, wherein the thickness of the first NdFeB layer is 35 nm; depositing a PrZn layer on the first NdFeB layer by taking the PrZn alloy as a target material, wherein the thickness of the PrZn layer is 9 nm; depositing a second NdFeB layer on the PrZn layer by taking the NdFeB as a target material, wherein the thickness of the second NdFeB layer is 18 nm; and depositing a CaB6 layer on the second NdFeB layer by taking CaB6 as a target, wherein the thickness of the CaB6 layer is 45 nm. Wherein the nominal chemical formula of the CuGe alloy is Cu100-xGexX ═ 9.5, and wherein the deposition of the CuGe layer on the glass substrate is carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 2.5Pa, the sputtering power is 140W, the sputtering voltage is 450V, and the substrate temperature is 380 ℃. Wherein the nominal chemical formula of the CoPbMn alloy target material is CoaPbbMn100-a-bAnd a-5 and b-35, and wherein depositing the CoPbMnO layer on the CuGe layer is performed under the following conditions: the method adopts a reactive radio frequency magnetron sputtering method, the sputtering atmosphere is oxygen, the sputtering pressure is 5.5Pa, the sputtering power is 450W, the sputtering voltage is 550V, and the substrate temperature is 380 ℃. Depositing a DyZn layer on the CoPbMnO layerThe following conditions were used: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 4.5Pa, the sputtering power is 180W, the sputtering voltage is 280V, and the substrate temperature is 480 ℃. The deposition of the first NdFeB layer on the DyZn layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 4.5Pa, the sputtering power is 230W, the sputtering voltage is 280V, and the substrate temperature is 280 ℃. The deposition of the PrZn layer on the first NdFeB layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 4.5Pa, the sputtering power is 90W, the sputtering voltage is 180V, and the substrate temperature is 330 ℃. The deposition of the second NdFeB layer on the PrZn layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 4.5Pa, the sputtering power is 220W, the sputtering voltage is 280V, and the substrate temperature is 580 ℃. The deposition of the CaB6 layer on the second NdFeB layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 4.5Pa, the sputtering power is 140W, the sputtering voltage is 140V, and the substrate temperature is 330 ℃.
Comparative example 1
The different steps or parameters from example 1 are: no CuGe layer was deposited on the glass substrate.
Comparative example 2
The different steps or parameters from example 1 are: no CoPbMnO layer was deposited on the CuGe layer.
Comparative example 3
The different steps or parameters from example 1 are: no DyZn layer was deposited on the CoPbMnO layer.
Comparative example 4
The different steps or parameters from example 1 are: no second NdFeB layer was deposited over the PrZn layer.
Comparative example 5
The different steps or parameters from example 1 are: the thickness of the CuGe layer is 15-30 nm.
Comparative example 6
The different steps or parameters from example 1 are: the thickness of the CoPbMnO layer is 20-40 nm.
Comparative example 7
The different steps or parameters from example 1 are: the thickness of the CaB6 layer is 30-50 nm.
Comparative example 8
The different steps or parameters from example 1 are: the nominal chemical formula of the CuGe alloy is Cu100-xGex，x＝15。
Comparative example 9
The different steps or parameters from example 1 are: the deposition of the CuGe layer on the glass substrate is carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 2.5Pa, the sputtering power is 200W, the sputtering voltage is 200V, and the substrate temperature is 200 ℃.
Comparative example 10
The different steps or parameters from example 1 are: the nominal chemical formula of the CoPbMn alloy target material is CoaPbbMn100-a-b，a＝2，b＝10。
Comparative example 11
The different steps or parameters from example 1 are: the deposition of the CoPbMnO layer on the CuGe layer was carried out under the following conditions: adopting a reactive radio frequency magnetron sputtering method, wherein the sputtering atmosphere is oxygen, the sputtering pressure is 5Pa, the sputtering power is 250W, the sputtering voltage is 300V, and the substrate temperature is 250 ℃.
Comparative example 12
The different steps or parameters from example 1 are: the deposition of the DyZn layer on the CoPbMnO layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3Pa, the sputtering power is 250W, the sputtering voltage is 400V, and the substrate temperature is 600 ℃.
Comparative example 13
The different steps or parameters from example 1 are: the deposition of the first NdFeB layer on the DyZn layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3Pa, the sputtering power is 300W, the sputtering voltage is 350V, and the substrate temperature is 350 ℃.
Comparative example 14
The different steps or parameters from example 1 are: the deposition of the PrZn layer on the first NdFeB layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3Pa, the sputtering power is 150W, the sputtering voltage is 250V, and the substrate temperature is 400 ℃.
Comparative example 15
The different steps or parameters from example 1 are: the deposition of the second NdFeB layer on the PrZn layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3Pa, the sputtering power is 300W, the sputtering voltage is 350V, and the substrate temperature is 450 ℃.
Comparative example 16
The different steps or parameters from example 1 are: the deposition of the CaB6 layer on the second NdFeB layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3Pa, the sputtering power is 200W, the sputtering voltage is 200V, and the substrate temperature is 200 ℃.
Examples 1 to 5 and comparative examples 1 to 16 were tested for saturation magnetization (unit is emu/cm)3) And coercivity (in Oe), the test was performed using a VSM known in the art, and the results are shown in table 1.
TABLE 1
Figure BDA0001756305790000121
Figure BDA0001756305790000131
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.

Claims (8)

1. CaB with strong ferromagnetism6The preparation method of the film is characterized by comprising the following steps: the CaB with strong ferromagnetism6The preparation method of the film comprises the following steps:
preparing a glass substrate;
depositing a CuGe layer on the glass substrate by taking a CuGe alloy as a target, wherein the thickness of the CuGe layer is 15-30 nm;
depositing a CoPbMnO layer on the CuGe layer by taking CoPbMn alloy as a target, wherein the thickness of the CoPbMnO layer is 20-40 nm;
depositing a DyZn layer on the CoPbMnO layer by taking DyZn alloy as a target, wherein the thickness of the DyZn layer is 10-30 nm;
depositing a first NdFeB layer on the DyZn layer by taking NdFeB as a target material, wherein the thickness of the first NdFeB layer is 20-40 nm;
depositing a PrZn layer on the first NdFeB layer by taking a PrZn alloy as a target, wherein the thickness of the PrZn layer is 5-10 nm;
depositing a second NdFeB layer on the PrZn layer by taking NdFeB as a target material, wherein the thickness of the second NdFeB layer is 10-20 nm; and
with CaB6Depositing CaB on the second NdFeB layer as a target material6Layer, wherein said CaB6The layer thickness is 30-50 nm.
2. CaB with strong ferromagnetism according to claim 16The preparation method of the film is characterized by comprising the following steps: wherein the nominal chemical formula of the CuGe alloy is Cu100-xGexAnd x is 8-10, and wherein depositing a layer of CuGe on the glass substrate is performed under the following conditions: the radio frequency magnetron sputtering method is adopted, the sputtering atmosphere is argon, the sputtering pressure is 2-3Pa, the sputtering power is 100-150W, the sputtering voltage is 300-500V, and the substrate temperature is 300-400 ℃.
3. CaB with strong ferromagnetism according to claim 16A method for preparing a thin film, which comprises the following steps,the method is characterized in that: wherein the nominal chemical formula of the CoPbMn alloy target material is CoaPbbMn100-a-bA-3-6, b-20-40, and wherein depositing a CoPbMnO layer on the CuGe layer is performed under the following conditions: the reactive radio frequency magnetron sputtering method is adopted, the sputtering atmosphere is oxygen, the sputtering pressure is 5-6Pa, the sputtering power is 500W-.
4. CaB with strong ferromagnetism according to claim 16The preparation method of the film is characterized by comprising the following steps: depositing a DyZn layer on the CoPbMnO layer is performed under the following conditions: the radio frequency magnetron sputtering method is adopted, the sputtering atmosphere is argon, the sputtering pressure is 3-5Pa, the sputtering power is 150-200W, the sputtering voltage is 200-300V, and the substrate temperature is 400-500 ℃.
5. CaB with strong ferromagnetism according to claim 16The preparation method of the film is characterized by comprising the following steps: the deposition of the first NdFeB layer on the DyZn layer was carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3-5Pa, the sputtering power is 150-250W, the sputtering voltage is 200-300V, and the substrate temperature is 150-300 ℃.
6. CaB with strong ferromagnetism according to claim 16The preparation method of the film is characterized by comprising the following steps: the deposition of the PrZn layer on the first NdFeB layer is carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3-5Pa, the sputtering power is 50-100W, the sputtering voltage is 150-200V, and the substrate temperature is 250-350 ℃.
7. CaB with strong ferromagnetism according to claim 16The preparation method of the film is characterized by comprising the following steps: depositing a second NdFeB layer over the PrZn layer is performed under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3-5Pa, the sputtering power is 150-250W, the sputtering voltage is 200-300V, and the substrate temperature is500-600℃。
8. CaB with strong ferromagnetism according to claim 16The preparation method of the film is characterized by comprising the following steps: depositing CaB on the second NdFeB layer6The layers were carried out under the following conditions: adopting a radio frequency magnetron sputtering method, wherein the sputtering atmosphere is argon, the sputtering pressure is 3-5Pa, the sputtering power is 100-150W, the sputtering voltage is 100-150V, and the substrate temperature is 250-350 ℃.
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