Selectively oxidized multilayer ternary molybdenum alloy film and preparation method thereof
By preparing selectively oxidized multilayer ternary molybdenum alloy thin films, the problems of insufficient high-temperature stability and conductivity of Mo thin films were solved, and the stability and conductivity of the films at high temperatures were improved.
Patent Information
- Application Number
- CN202511762931.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-27
- Publication Date
- 2026-02-27
AI Technical Summary
Existing Mo films exhibit poor stability and high brittleness at high temperatures, failing to meet the application requirements of fields such as high-performance integrated circuits and back contact layers for solar cells.
Selective oxidation of multilayer ternary molybdenum alloy thin films, comprising Mo, Ta, Ni, Al, Cr and Nb, was employed. Multilayer molybdenum alloy thin films were prepared by vapor deposition and annealing to form a transparent Ta oxide protective layer, thereby improving the high-temperature stability and conductivity of the thin film.
It significantly improves the high-temperature stability and conductivity of the thin film, enhances its oxidation resistance and corrosion resistance, and reduces its resistivity.
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Figure CN121575286A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of molybdenum-based alloy thin film technology, specifically relating to a selective oxidation multilayer ternary molybdenum alloy thin film and its preparation method. Background Technology
[0002] Refractory metal thin film materials, due to the need for internal electron (layer) reorganization, possess a series of physical properties such as high melting point, hardness, strength, good ductility, corrosion resistance, and wear resistance, giving them significant advantages and a prominent position in high-performance integrated circuits and large-scale PCB manufacturing. Among these, molybdenum (Mo)-based thin films, with their excellent electrical conductivity, low thermal expansion, high melting point, and unique optical and mechanical properties, are widely used as gate materials in integrated circuits and back contact layers in solar cells. These characteristics make them indispensable in advanced fields such as high-performance integrated circuits, large-scale PCB manufacturing, and thin-film transistor liquid crystal displays (TFT-LCDs).
[0003] However, single Mo thin films cannot currently meet application requirements. This is because single Mo thin films are relatively brittle and prone to fracture under external loads. Furthermore, Mo oxides are volatile and have poor stability at high temperatures, limiting the reliability of the films during service. With the continuous development of the electronics and information field, thin films now exhibit multi-field coupling characteristics, leading to increasingly complex service environments.
[0004] Therefore, ensuring the high-temperature stability of molybdenum alloy thin films while maintaining good electrical conductivity is an important issue that urgently needs to be studied. Summary of the Invention
[0005] In order to overcome the shortcomings of the prior art, the present invention aims to provide a selective oxidation multilayer ternary molybdenum alloy thin film and its preparation method, so as to solve the technical problem that existing Mo thin films are difficult to have good high-temperature stability and conductivity to meet different working requirements.
[0006] To achieve the above objectives, the present invention employs the following technical solution: A selectively oxidized multilayer molybdenum alloy film, comprising, by mass percentage: Mo: 70.0%–75.0%, Ta: 15.0%–20.0%, Ni: 1.0%–5.0%, Al: 1.0%–5.0%, Cr: 1.0%–5.0%, Nb: 1.0%–5.0%, with the balance being unavoidable impurities, the sum of the mass percentages of the above components being 100%.
[0007] Optionally, the impurity content is no more than 0.05%.
[0008] Optional, the following steps may be included: S1: Clean the Mo target, Ta target, Ni target, Al target, Cr target, Nb target and substrate for later use; S2: A film is deposited on the substrate using a vapor deposition method. The deposition rate of the Mo target is fixed. The deposition rates of the Ta, Ni, Al, Cr and Nb targets are calculated based on the stoichiometry. The deposition time is calculated based on the deposition rate of different target materials and the film thickness. The film deposition process then begins. S3: The deposited film is annealed in a vacuum furnace at a temperature of 500-700℃ for 4 hours.
[0009] Optionally, in S2: the deposition rate of the Mo target is 20 nm / min, the deposition rate of the Ta target is 5.9–8.3 nm / min, the deposition rate of the Ni target is 1.1–2.2 nm / min, the deposition rate of the Al target is 1.1–2.0 nm / min, the deposition rate of the Cr target is 1.0–1.7 nm / min, the deposition rate of the Nb target is 0.6–1.2 nm / min, and the deposition time is 2966–3470 s.
[0010] Optionally, the equipment for the vapor deposition method is a closed-field unbalanced magnetron sputtering system; The vacuum level in the system drops to <4×10 -5 After Pa, inert gas is introduced; the rotational speed of the workpiece holder is set to 8-10 rpm, and a bias voltage of -65V is applied to the substrate.
[0011] Optionally, the inert gas introduced is Ar gas, and the flow rate is 15 sccm.
[0012] Optionally, during the coating process, the vacuum level inside the vacuum chamber is maintained at 4×10⁻⁶. -3 Below Pa; temperature between 40 and 80℃.
[0013] Optionally, the purity of the Mo, Ta, Ni, Al, Cr, and Nb targets is 99.99%, and the cleaned targets are placed in a vacuum chamber and cleaned by argon ion bombardment for 10 minutes; the ultrasonic cleaning power of the substrate material is 45W, and the cleaning time is 15 minutes.
[0014] Optionally, the film thickness is 100 nm.
[0015] Optionally, in step S3, the vacuum degree of the vacuum furnace used for annealing is less than 1×10⁻⁶. -3 Pa.
[0016] Compared with the prior art, the present invention has the following beneficial effects: The selectively oxidized multilayer molybdenum alloy thin films of this invention utilize Ta, which possesses high melting point, high density, resistance to oxidation, and good toughness. Adding Ta to the Mo film significantly reduces the ductile / brittle transition temperature of Mo, increases the recrystallization temperature, improves room-temperature plasticity and high-temperature strength, and enhances oxidation resistance. Ni has a stabilizing effect on the BCC structure of Mo, and its strong d-electron orbital contribution may broaden the d-bandwidth of the Mo-Ta matrix, effectively increasing the DOS near the Fermi level. This modification simultaneously suppresses lattice distortion through solid solution strengthening, thereby reducing electron scattering. Therefore, a higher binding energy is obtained, effectively improving stability and reducing conductivity. The passivation film formed by Al and Cr further improves the corrosion resistance and stability of the film, while the addition of the refractory element Nb increases the high-temperature stability of the film and effectively reduces the diffusion barrier performance and resistivity. Ternary alloy thin films such as Mo-Ta-Ni, Mo-Ta-Al, Mo-Ta-Cr, and Mo-Ta-V are prepared sequentially. Attached Figure Description
[0017] The accompanying drawings are provided to further illustrate the present disclosure and form part of the specification. They are used together with the following detailed description to explain the present disclosure, but do not constitute a limitation thereof. In the drawings: Figure 1 Transmission electron microscope (TEM) images and elemental energy dispersive spectroscopy (EDS) spectra of the microstructure of the selectively oxidized multilayer molybdenum alloy thin film prepared in this invention. Figure 2 These are the resistivity test results. Detailed Implementation
[0018] To enable those skilled in the art to understand the features and effects of the present invention, the terms and expressions used in the specification and claims are explained and defined in general below. Unless otherwise specified, all technical and scientific terms used herein have the ordinary meaning understood by those skilled in the art regarding the present invention, and in case of conflict, the definitions in this specification shall prevail.
[0019] The theories or mechanisms described and disclosed herein, whether right or wrong, should not in any way limit the scope of the invention, that is, the contents of the invention can be implemented without being limited by any particular theory or mechanism.
[0020] In this document, all features defined by numerical ranges or percentage ranges, such as numerical values, quantities, contents, and concentrations, are for the sake of brevity and convenience only. Accordingly, descriptions of numerical ranges or percentage ranges should be considered as covering and specifically disclosing all possible sub-ranges and individual numerical values (including integers and fractions) within those ranges.
[0021] In this article, unless otherwise specified, “contains,” “includes,” “containing,” “has,” or similar terms cover the meanings of “composed of” and “mainly composed of,” for example, “A contains a” covers the meanings of “A contains a and others” and “A contains only a.”
[0022] For the sake of brevity, not all possible combinations of the technical features in each implementation scheme or embodiment are described herein. Therefore, as long as there is no contradiction in the combination of these technical features, the technical features in each implementation scheme or embodiment can be combined arbitrarily, and all possible combinations should be considered within the scope of this specification.
[0023] This invention discloses a selective oxidation method for multilayer ternary molybdenum alloy thin films and its preparation method, belonging to the field of molybdenum-based alloy thin film technology. The molybdenum alloy thin films disclosed in this invention are ternary alloy thin films such as Mo-Ta-Ni, Mo-Ta-Al, Mo-Ta-Cr, and Mo-Ta-V. Multilayer molybdenum alloy thin films are formed by adding metallic elements Ta, Ni, Al, Cr, and Nb to the Mo film. Ta preferentially oxidizes to form a transparent Ta oxide scale, which acts as a protective layer and further enhances the corrosion resistance of the film. Ni, as a transition metal, can improve the electron density of the film, thereby improving its electrical properties and thermal stability. Al and Cr directly participate in the formation of the surface passivation film, thus improving the corrosion resistance of the alloy film. Nb, as a refractory metal, can maintain the stability of the passivation film. By adjusting the deposition rate and deposition time of different targets, the content of Ta, Ni, Al, Cr, and Nb elements in the film is controlled, followed by vacuum annealing, to prepare multilayer molybdenum alloy thin films with excellent high-temperature stability and electrical conductivity.
[0024] This invention discloses a selectively oxidized multilayer molybdenum alloy thin film, comprising, by mass percentage: Mo: 70.0%–75.0%, Ta: 15.0%–20.0%, Ni: 1.0%–5.0%, Al: 1.0%–5.0%, Cr: 1.0%–5.0%, Nb: 1.0%–5.0%, with the balance being unavoidable impurities. The sum of the mass percentages of the above components is 100%. The impurity content is no greater than 0.05%.
[0025] This invention also discloses a method for preparing the above-mentioned selectively oxidized multilayer molybdenum alloy thin film, comprising the following steps: S1: The rectangular Mo, Ta, Ni, Al, Cr and Nb targets with dimensions of 330×145×10mm were sandblasted and cleaned with acetone and anhydrous ethanol, respectively. S2: The appropriately cut substrate material is ultrasonically cleaned in acetone (monocrystalline silicon and glass slide substrate) and anhydrous ethanol (polyimide substrate), then dried and clamped on the workpiece holder in the center of the vacuum chamber to remove surface oil. S3: Place the cleaned target into the closed-field unbalanced magnetron sputtering system (MSIP016), evacuate the vacuum, and then introduce inert gas; S4: During the deposition process, the deposition rate of the Mo target is fixed, and then the deposition rates of the Ta, Ni, Al, Cr and Nb targets are calculated based on the stoichiometry. The deposition time is further calculated based on the deposition rate and film thickness of different target materials, and the coating process is started according to the calculated parameters. S5: During the experiment, the workpiece holder rotation speed needs to be set to 8-10 rpm in advance, and a -65V bias voltage needs to be applied to the substrate. During the coating process, the vacuum level in the vacuum chamber should be maintained at 4×10⁻⁶. -3 Below Pa.
[0026] S6: The deposited film is annealed in a vacuum furnace at a temperature of 500℃-700℃ for 4 hours.
[0027] Furthermore, in S1, the purity of the Mo, Ta, Ni, Al, Cr and Nb targets used is 99.99%, and the cleaned targets need to be placed in a vacuum chamber and bombarded with argon ions for 10 minutes.
[0028] Furthermore, in S2, the ultrasonic cleaning power of the substrate material is 45W, and the cleaning time is not less than 15 minutes; Furthermore, the vacuum level in the vacuum chamber of S3 is reduced to <4×10⁻⁶. -5 After Pa, an inert gas is introduced. Further, in S3, the inert gas introduced is Ar (purity 99.9%), and the flow rate is 15 sccm.
[0029] Furthermore, in S4, when calculating the deposition rate and deposition time, the expected film thickness is 100 nm, and the actual composition of the film needs to be controlled to have an error of less than 5% compared with the nominal composition; furthermore, in S4, the Mo target deposition rate is fixed at 20 nm / min during the deposition process.
[0030] Furthermore, in S5, the coating process is carried out at room temperature, but due to the change in target power, the temperature of the vacuum chamber needs to be controlled between 40-80°C during the thin film growth process.
[0031] Furthermore, in S6, the vacuum level of the vacuum furnace used for annealing the film layer is required to be less than 1×10⁻⁶. -3 Pa.
[0032] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.
[0033] The following examples use instruments and equipment conventional in the art. Experimental methods in the following examples, unless otherwise specified, are generally performed under conventional conditions or as recommended by the manufacturer. All raw materials used in the following examples are conventional commercially available products with specifications conventional in the art. In this specification and the following examples, unless otherwise specified, "%" refers to weight percentage, "parts" refers to parts by weight, and "ratio" refers to weight proportion.
[0034] Example 1: A method for preparing a selectively oxidized multilayer molybdenum alloy thin film includes the following steps: S1: The rectangular Mo, Ta, Ni, Al, Cr and Nb targets with dimensions of 330×145×10mm were sandblasted for 10 minutes and then wiped clean with acetone and anhydrous ethanol respectively. S2: The appropriately cut substrate material is ultrasonically cleaned in acetone (monocrystalline silicon and glass slide substrate) and anhydrous ethanol (polyimide substrate), then dried and clamped on the workpiece holder in the center of the vacuum chamber. S3: Place the cleaned target material into a UDP450 magnetron sputtering ion plating apparatus and evacuate to a vacuum level of 4×10⁻⁶. -5 After Pa, inert gas Ar with a purity of 99.9% is introduced at a flow rate of 15 sccm. S4: Calculate the deposition rate and deposition time based on the film thickness, and set the coating process parameters. During the deposition process, the deposition rate of Mo target is fixed at 20 nm / min, Ta target at 6.6 nm / min, Ni target at 1.4 nm / min, Al target at 1.2 nm / min, Cr target at 1.1 nm / min, Nb target at 0.6 nm / min, and the deposition time is 3383 s. S5: During the experiment, the workpiece holder rotation speed was set to 8 rpm, and a -65V bias voltage was applied to the substrate. During the coating process, the vacuum level in the vacuum chamber was maintained at 4 × 10⁻⁶. -3 Below Pa, the temperature inside the vacuum chamber is controlled at 40-80℃.
[0035] S6: Anneal the deposited film at 500℃ for 4 hours in a vacuum furnace.
[0036] Example 2: A method for preparing a selectively oxidized multilayer molybdenum alloy thin film includes the following steps: S1: The rectangular Mo, Ta, Ni, Al, Cr and Nb targets with dimensions of 330×145×10mm were sandblasted for 10 minutes and then wiped clean with acetone and anhydrous ethanol respectively. S2: The appropriately cut substrate material is ultrasonically cleaned in acetone (monocrystalline silicon and glass slide substrate) and anhydrous ethanol (polyimide substrate), then dried and clamped on the workpiece holder in the center of the vacuum chamber. S3: Place the cleaned target material into a UDP450 magnetron sputtering ion plating apparatus and evacuate to a vacuum level of 4×10⁻⁶. -5 After Pa, inert gas Ar with a purity of 99.9% is introduced at a flow rate of 15 sccm. S4: Calculate the deposition rate and deposition time based on the film thickness, and set the coating process parameters. During the deposition process, the deposition rate of Mo target is fixed at 20 nm / min, Ta target at 5.9 nm / min, Ni target at 1.8 nm / min, Al target at 1.7 nm / min, Cr target at 1.5 nm / min, Nb target at 1.1 nm / min, and the deposition time is 3470 s. S5: During the experiment, the workpiece holder rotation speed was set to 8 rpm, and a -65V bias voltage was applied to the substrate. During the coating process, the vacuum level in the vacuum chamber was maintained at 4 × 10⁻⁶. -3 Below Pa, the temperature inside the vacuum chamber is controlled at 40-80℃.
[0037] S6: Anneal the deposited film at 550℃ for 4 hours in a vacuum furnace.
[0038] Example 3: A method for preparing a selectively oxidized multilayer molybdenum alloy thin film includes the following steps: S1: The rectangular Mo, Ta, Ni, Al, Cr and Nb targets with dimensions of 330×145×10mm were sandblasted for 10 minutes and then wiped clean with acetone and anhydrous ethanol respectively. S2: The appropriately cut substrate material is ultrasonically cleaned in acetone (monocrystalline silicon and glass slide substrate) and anhydrous ethanol (polyimide substrate), then dried and clamped on the workpiece holder in the center of the vacuum chamber. S3: Place the cleaned target material into a UDP450 magnetron sputtering ion plating apparatus and evacuate to a vacuum level of 4×10⁻⁶. -5After Pa, inert gas Ar with a purity of 99.9% is introduced at a flow rate of 15 sccm. S4: Calculate the deposition rate and deposition time based on the film thickness, and set the coating process parameters. During the deposition process, the deposition rate of Mo target is fixed at 20 nm / min, the deposition rate of Ta target is 7.3 nm / min, the deposition rate of Ni target is 1.1 nm / min, the deposition rate of Al target is 1.1 nm / min, the deposition rate of Cr target is 1.0 nm / min, the deposition rate of Nb target is 0.8 nm / min, and the deposition time is 3295 s. S5: During the experiment, the workpiece holder rotation speed was set to 8 rpm, and a -65V bias voltage was applied to the substrate. During the coating process, the vacuum level in the vacuum chamber was maintained at 4 × 10⁻⁶. -3 Below Pa, the temperature inside the vacuum chamber is controlled at 40-80℃.
[0039] S6: Anneal the deposited film at 600℃ for 4 hours in a vacuum furnace.
[0040] Example 4: A method for preparing a selectively oxidized multilayer molybdenum alloy thin film includes the following steps: S1: The rectangular Mo, Ta, Ni, Al, Cr and Nb targets with dimensions of 330×145×10mm were sandblasted for 10 minutes and then wiped clean with acetone and anhydrous ethanol respectively. S2: The appropriately cut substrate material is ultrasonically cleaned in acetone (monocrystalline silicon and glass slide substrate) and anhydrous ethanol (polyimide substrate), then dried and clamped on the workpiece holder in the center of the vacuum chamber. S3: Place the cleaned target material into a UDP450 magnetron sputtering ion plating apparatus and evacuate to a vacuum level of 4×10⁻⁶. -5 After Pa, inert gas Ar with a purity of 99.9% is introduced at a flow rate of 15 sccm. S4: Calculate the deposition rate and deposition time based on the film thickness, and set the coating process parameters. During the deposition process, the deposition rate of Mo target is fixed at 20 nm / min, Ta target at 8.1 nm / min, Ni target at 2.1 nm / min, Al target at 1.8 nm / min, Cr target at 1.6 nm / min, Nb target at 1.2 nm / min, and the deposition time is 3207 s. S5: During the experiment, the workpiece holder rotation speed was set to 8 rpm, and a -65V bias voltage was applied to the substrate. During the coating process, the vacuum level in the vacuum chamber was maintained at 4 × 10⁻⁶. -3 Below Pa, the temperature inside the vacuum chamber is controlled at 40-80℃.
[0041] S6: Anneal the deposited film at 650℃ for 4 hours in a vacuum furnace.
[0042] Example 5 A method for preparing a selectively oxidized multilayer molybdenum alloy thin film includes the following steps: S1: The rectangular Mo, Ta, Ni, Al, Cr and Nb targets with dimensions of 330×145×10mm were sandblasted for 10 minutes and then wiped clean with acetone and anhydrous ethanol respectively. S2: The appropriately cut substrate material is ultrasonically cleaned in acetone (monocrystalline silicon and glass slide substrate) and anhydrous ethanol (polyimide substrate), then dried and clamped on the workpiece holder in the center of the vacuum chamber. S3: Place the cleaned target material into a UDP450 magnetron sputtering ion plating apparatus and evacuate to a vacuum level of 4×10⁻⁶. -5 After Pa, inert gas Ar with a purity of 99.9% is introduced at a flow rate of 15 sccm. S4: Calculate the deposition rate and deposition time based on the film thickness, and set the coating process parameters. During the deposition process, the deposition rate of Mo target is fixed at 20 nm / min, Ta target at 8.3 nm / min, Ni target at 2.2 nm / min, Al target at 2.0 nm / min, Cr target at 1.7 nm / min, Nb target at 0.9 nm / min, and the deposition time is 2966 s. S5: During the experiment, the workpiece holder rotation speed was set to 8 rpm, and a -65V bias voltage was applied to the substrate. During the coating process, the vacuum level in the vacuum chamber was maintained at 4 × 10⁻⁶. -3 Below Pa, the temperature inside the vacuum chamber is controlled at 40-80℃.
[0043] S6: Anneal the deposited film at 700℃ for 4 hours in a vacuum furnace.
[0044] The microstructure morphology of the selectively oxidized multilayer molybdenum alloy thin film obtained in Example 1 was characterized using transmission electron microscopy. Figure 1 The cross-sectional images of the thin film show that the surface of the alloy film is relatively smooth and flat. The absence of delamination at high temperatures indicates good high-temperature stability, exhibiting characteristics of sputtered deposited films. Simultaneously, multilayer oxide delamination is clearly observed, including tantalum oxide, tantalum-rich, molybdenum oxide, and molybdenum-rich layers. Figure 2 The room temperature resistivity of the thin film was tested. The room temperature resistivity of the Mo-Ta-Re thin film decreased with increasing annealing temperature, indicating that it has good electrical conductivity.
[0045] The above content is only for illustrating the technical concept of the present invention and should not be construed as limiting the scope of protection of the present invention. Any modifications made to the technical solution based on the technical concept proposed in this invention shall fall within the scope of protection of the claims of this invention.
Claims
1. A selectively oxidized multilayer molybdenum alloy thin film characterized by, The components include, in percentage by mass: Mo: 70.0-75.0%, Ta: 15.0-20.0%, Ni: 1.0-5.0%, Al: 1.0-5.0%, Cr: 1.0-5.0%, Nb: 1.0-5.0%, and the balance being inevitable impurities, with the sum of the percentages by mass of the above components being 100%.
2. The selectively oxidized multilayer molybdenum alloy film of claim 1, wherein, The impurity content is not more than 0.05%.
3. The method of producing a selectively oxidized multilayer molybdenum alloy film according to claim 1 or 2, characterized in that, The method comprises the following steps: S1: cleaning Mo target, Ta target, Ni target, Al target, Cr target, Nb target and substrate for standby; S2: depositing a film on the substrate by a vapor deposition method, fixing the deposition rate of the Mo target, calculating the deposition rates of the Ta target, Ni target, Al target, Cr target and Nb target according to the stoichiometric ratio, calculating the deposition time according to the deposition rates of different targets and the film thickness, and starting the film deposition process; S3: annealing the deposited film in a vacuum furnace, with the annealing temperature being 500-700 DEG C and the holding time being 4h.
4. The method of claim 3, wherein the selective oxidation of the multilayered molybdenum alloy thin film is performed by a process selected from the group consisting of thermal oxidation, anodic oxidation, and a combination thereof. In S2, the deposition rate of the Mo target is 20nm / min, the deposition rate of the Ta target is 5.9-8.3nm / min, the deposition rate of the Ni target is 1.1-2.2nm / min, the deposition rate of the Al target is 1.1-2.0nm / min, the deposition rate of the Cr target is 1.0-1.7nm / min, the deposition rate of the Nb target is 0.6-1.2nm / min, and the deposition time is 2966-3470s.
5. The method of claim 3, wherein the selective oxidation of the multilayered molybdenum alloy thin film is performed by a process selected from the group consisting of thermal oxidation, anodic oxidation, and a combination thereof. The equipment of the vapor deposition method is a closed field unbalanced magnetron sputtering system. The vacuum degree in the system is reduced to <4x10 -5 After that, inert gas is introduced; the rotating speed of the workpiece holder is set to 8-10 rmp, and a bias of -65 V is loaded on the substrate.
6. The method for preparing selectively oxidized multilayer molybdenum alloy thin films according to claim 5, characterized in that, The inert gas is Ar gas, and the flow rate is 15sccm.
7. The method of claim 3, wherein the selective oxidation of the multilayered molybdenum alloy thin film is performed by a process selected from the group consisting of thermal oxidation, anodic oxidation, and a combination thereof. During the coating process, the vacuum degree in the vacuum cavity is kept at 4x10 -3 Pa; the temperature is between 40-80℃.
8. The method for preparing selectively oxidized multilayer molybdenum alloy thin films according to claim 3, characterized in that, The purity of the Mo target, Ta target, Ni target, Al target, Cr target and Nb target is 99.99%, and the cleaned target is placed in the vacuum chamber and cleaned by argon ion bombardment for 10min; the ultrasonic cleaning power of the substrate material is 45W, and the cleaning time is 15min.
9. The method of claim 3, wherein the selective oxidation of the multilayered molybdenum alloy thin film is performed by a process selected from the group consisting of thermal oxidation, anodic oxidation, and a combination thereof. The film thickness is 100nm.
10. The method of claim 3 wherein the selectively oxidized multilayer molybdenum alloy film is prepared by the steps of: The vacuum degree of the vacuum furnace for annealing in the S3 is less than 1x10 -3 Pa.