A zr / mo metal multilayer film and a method of manufacturing the same

Abstract

The application discloses a Zr / Mo metal multilayer film, and the Zr / Mo metal multilayer film is a multilayer film with preferred orientation, and the multilayer film comprises Zr atomic layers and Mo atomic layers; the Zr atomic layers and the Mo atomic layers are alternately distributed, there is intermixing between the Zr atomic layers and the Mo atomic layers, and the layer thickness of the Zr atomic layers is equal to that of the Mo atomic layers. The preparation method of the Zr / Mo metal multilayer film specifically comprises the following steps: step 1, cleaning and drying the surface of a single crystal Si substrate; step 2, feeding the substrate into a magnetron sputtering film coating chamber and then performing vacuum pumping; step 3, performing ion bombardment cleaning on the substrate, and then depositing the Zr / Mo metal multilayer film on the substrate by magnetron sputtering; and step 4, vacuum cooling the substrate obtained in step 3, and taking out the sample obtained by sputtering when the temperature of the cavity is reduced to below 50 DEG C. The technical effect of the application is that the comprehensive mechanical properties of the Zr / Mo metal multilayer film are effectively improved, and the prepared interface structure is clear, the organization is dense and uniform, and the performance is excellent.

Description

Technical Field

[0001] The present invention relates to the technical field of metal structural materials, in particular to a Zr / Mo metal multilayer film and a preparation method thereof. Background Art

[0002] Social and economic development is accompanied by significant energy consumption, yet traditional fossil fuel reserves are limited. Consequently, the development of new clean energy sources has become an international consensus, with nuclear energy being one of the clean energy sources with the greatest potential. Nuclear reactors generate significant amounts of radioactive materials during operation. Nuclear fuel cladding, the primary safety barrier, is crucial for safe and stable reactor operation. Its material selection and structural integrity are crucial.

[0003] Zr and Zr alloys are widely used as fuel cladding materials for nuclear reactors due to their outstanding advantages, such as a small thermal neutron absorption cross-section and excellent corrosion resistance. However, in the event of a loss of coolant (LOCA), the temperature in the core rises sharply due to the loss of coolant, triggering a zirconium-water reaction that leads to a core melt and a hydrogen explosion. The technology for preparing a coating on the surface of the Zr alloy cladding material substrate can isolate the substrate from high-temperature water vapor and improve surface hardness and radiation resistance without changing the service performance of the substrate itself. The service conditions within the reactor are harsh, so the design and preparation of radiation-resistant coatings with excellent combined performance and outstanding mechanical properties are crucial to the long-term safe and stable service of nuclear reactors.

[0004] Mo is considered a candidate material for nuclear fuel cladding due to its excellent high-temperature strength, strong neutron irradiation resistance, and creep resistance. Furthermore, the numerous grain boundaries and heterogeneous interfaces within the multilayer film act as effective traps for high-energy ions, absorbing and eliminating radiation defects within the material, effectively improving the coating's radiation resistance. Therefore, the present invention utilizes Zr and Mo to form a multilayer film, developing a radiation-resistant coating with a dense and uniform microstructure and excellent mechanical properties. Summary of the Invention

[0005] The purpose of the present invention is to provide a Zr / Mo metal multilayer film and a preparation method thereof. The prepared Zr / Mo metal multilayer film has a dense and uniform microstructure and excellent mechanical strength, which can effectively improve and solve the safety problems of nuclear reactors.

[0006] To achieve the above object, the invention provides the following technical solution: a Zr / Mo metal multilayer film, wherein the Zr / Mo metal multilayer film is a multilayer film with preferred orientation, and the multilayer film includes Zr atomic layers and Mo atomic layers;

[0007] The Zr atomic layers and the Mo atomic layers are alternately distributed, there is intermixing between the Zr atomic layers and the Mo atomic layers, and the thicknesses of the Zr atomic layers and the Mo atomic layers are equal.

[0008] Preferably, the thickness of the Zr atomic layer and the Mo atomic layer are both 5-150 nm.

[0009] Preferably, the crystal grains in the Zr atomic layer and the Mo atomic layer are columnar nanocrystals.

[0010] Preferably, the nanoindentation hardness of the Zr / Mo metal multilayer film is in the range of 9.9-12.2 GPa, and when the layer thickness is large (h>20 nm), the hardness decreases as the layer thickness decreases.

[0011] The method for preparing the Zr / Mo metal multilayer film specifically comprises the following steps:

[0012] Step 1: Clean and dry the surface of the single crystal Si substrate;

[0013] Step 2: Place the substrate into the magnetron sputtering coating chamber and then evacuate it;

[0014] Step 3: After the substrate is cleaned by ion bombardment, Zr / Mo metal multilayer films are alternately deposited on the substrate by magnetron sputtering;

[0015] Step 4: The substrate obtained in step 3 is vacuum cooled, and the sputtered sample is taken out when the chamber temperature drops below 50°C.

[0016] Preferably, the specific steps of cleaning and drying in step 1 are:

[0017] The single crystal Si wafer was ultrasonically cleaned in acetone and alcohol for 10 minutes, and then dried. The roughness of the polished surface was less than 0.8 nm.

[0018] Preferably, the vacuum degree of the vacuum pumping in step 2 is less than 5×10 -4 Pa.

[0019] Preferably, the magnetron sputtering alternating deposition method in step 3 is: applying DC power to the Zr target and the Mo target separately to achieve alternating deposition.

[0020] Preferably, the purity of the Zr target is 99.99 wt%, the DC power supply current is 2.4 A, the purity of the Mo target is 99.99 wt%, the DC power supply current is 2.4 A, and the base plate rotation speed is 5 rad / min.

[0021] Preferably, the sputtering process of the magnetron sputtering alternating deposition is performed by continuously introducing Ar gas, and the deposition pressure is maintained at 1.2×10 -3Pa, a bias voltage of -65V was applied to the substrate during the deposition process, and the thickness of the single layer in the Zr / Mo metal multilayer film was adjusted by changing the sputtering time. The sputtering rates of Zr and Mo were 0.2nm / s and 0.32nm / s, respectively. The total thickness of the Zr / Mo metal multilayer film was 1.5μm. During the sputtering process, the substrate temperature increased with the extension of the sputtering time and did not exceed 100℃.

[0022] Compared with the prior art, the beneficial effects of the invention are:

[0023] 1. The Zr / Mo metal multilayer film and its preparation method, the prepared Zr / Mo metal multilayer film, the Zr layer and the Mo layer both show nano-columnar crystal growth, and have two different types of preferred orientations, namely Zr (0002) / / Mo (110) and Zr / / Mo (110). The mismatch between these two orientations is 15.8% and 10.8%, respectively, resulting in a semi-coherent interface between the Zr and Mo layers. Since the mixing enthalpy between Zr and Mo is -6 kJ / mol, there is a small amount of intermixing between the Zr and Mo atomic layers, but their interface is straight and clear. The grain boundary / interface structure and the hindering effect of solid solution atoms on dislocation slip effectively improve the comprehensive mechanical properties of the Zr / Mo metal multilayer film. Its nanoindentation hardness ranges from 9.9 to 12.2 GPa, and when the layer thickness is large (h>20 nm), the hardness decreases with decreasing layer thickness, which is contrary to the "smaller, stronger" rule commonly found in multilayer films.

[0024] 2. The Zr / Mo metal multilayer film and its preparation method take advantage of the advantages of magnetron sputtering technology and control the single layer thickness of the multilayer film by changing the sputtering time to prepare a Zr / Mo metal multilayer film with a clear interface structure, dense and uniform organization and excellent performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 TEM cross-sectional photograph of the Zr / Mo metal multilayer film of the present invention;

[0026] Figure 2 This is the EDS energy spectrum scanning element distribution diagram of the Zr / Mo metal multilayer film of the present invention;

[0027] Figure 3 2 is the load-displacement curve of the Zr / Mo metal multilayer films with different layer thicknesses of the present invention;

[0028] Figure 4 These are the nanoindentation hardness results of Zr / Mo metal multilayer films with different layer thicknesses of the present invention. DETAILED DESCRIPTION

[0029] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0030] See also Figure 1-4 The invention provides a technical solution: a Zr / Mo metal multilayer film with equal Zr and Mo layer thicknesses, with a single layer thickness ranging from 5 to 150 nm, and nanocolumnar grains within the layer. Produced using magnetron sputtering alternating deposition, the multilayer film exhibits preferred orientation.

[0031] Figure 1 The TEM cross-sectional photograph of the Zr / Mo metal multilayer film of the present invention is shown in FIG. Figure 2 The EDS scanning element distribution diagram of the Zr / Mo metal multilayer film of the present invention is shown. Figure 3 The load-displacement curves of Zr / Mo metal multilayers with different single-layer thicknesses under nanoindentation are shown. Figure 4 The nanoindentation hardness of Zr / Mo metal multilayer films varies with the thickness of the film. According to the Zr / Mo metal multilayer film of the present invention, Zr atomic layers and Mo atomic layers are alternately distributed in the multilayer film. There is a small amount of intermixing between the two atomic layers, but the interface structure is straight and clear. The growth mode of the multilayer film is that the nanocolumnar crystals are confined to grow within the layer. There are two types of specific orientation relationships between the Zr layer and the Mo layer, namely Zr (0002) / / Mo (110) and Zr / / Mo (110). The Zr / Mo metal multilayer film of the present invention has very high strength / hardness, and the hardness decreases with decreasing layer thickness within a large layer thickness range (h>20 nm).

[0032] The present invention also provides a method for preparing a Zr / Mo metal multilayer film, comprising the following steps:

[0033] Step 1: Take a single-side polished single-crystal Si substrate, ultrasonically clean it in chemically pure acetone and ethanol for 10 minutes, and then quickly dry it with warm air to make its surface clean and free of stains and dust. The surface roughness of the single-crystal silicon substrate after ultrasonic treatment is less than 0.8nm.

[0034] Step 2: Fix the single crystal silicon substrate after ultrasonic cleaning to the base plate and evacuate until the back vacuum is less than 5×10 -4 Pa.

[0035] Step 3: After the substrate is cleaned by ion bombardment using a small current, a direct current power supply is applied to the Zr target and the Mo target separately to alternately deposit a Zr / Mo metal multilayer film on the substrate.

[0036] The purity of the Zr target was 99.99 wt%, the DC power supply current was 2.4 A, the purity of the Mo target was 99.99 wt%, the DC power supply current was 2.4 A, and the substrate speed was 5 rad / min. Ar gas was continuously introduced during the sputtering process, and the deposition pressure was maintained at 1.2×10 - 3 Pa, and a bias voltage of -65 V was applied to the substrate. The sputtering rates of Zr and Mo were 0.2 nm / s and 0.32 nm / s, respectively. The thickness of the single layer in the Zr / Mo metal multilayer film was adjusted by changing the sputtering time. The total thickness of the Zr / Mo metal multilayer film was 1.5 μm.

[0037] In step 4, the substrate temperature increases with increasing sputtering time due to the high-speed bombardment of sputtered atoms during deposition, but never exceeds 100°C. After deposition, the film is fully cooled in the high-vacuum coating chamber before removal, a process known as furnace annealing. This reduces the internal stress of the pre-coated film and prevents its surface from being oxidized by air.

[0038] The present invention uses magnetron sputtering technology to deposit Zr / Mo metal multilayer film on the surface of single crystal silicon wafer. The principle is to ionize Ar gas to generate Ar + Attracted by the cathode potential, ions are accelerated to bombard the cathode target (Zr and Mo). The sputtered target atoms are deposited in the opposite direction onto the anode substrate, forming a thin film. The moving electrons are subject to the Lorentz force in the magnetic field, causing their trajectory to bend or even spiral, increasing the number of collisions with the working gas. Consequently, this technology offers significant advantages: fast deposition rates, low substrate temperature rise, uniform and dense deposited films, and strong adhesion. Finally, the film is naturally cooled to room temperature in a high-vacuum coating chamber, allowing the deposited atoms to fully diffuse and form the final Zr / Mo metal multilayer film.

[0039] Example 1

[0040] A method for preparing a Zr / Mo metal multilayer film comprises the following steps:

[0041] Step 1: Take a single-side polished single-crystal Si substrate, ultrasonically clean it in chemically pure acetone and ethanol for 10 minutes, and then quickly dry it with warm air.

[0042] Step 2: Fix the single crystal silicon substrate after ultrasonic cleaning to the base plate and evacuate until the back vacuum is less than 5×10 -4 Pa.

[0043] Step 3: After the substrate is cleaned by ion bombardment using a small current, a direct current power supply is applied to the Zr target and the Mo target separately to alternately deposit a Zr / Mo metal multilayer film on the substrate.

[0044] The purity of the Zr target was 99.99 wt%, the DC power supply current was 2.4 A, the purity of the Mo target was 99.99 wt%, the DC power supply current was 2.4 A, and the substrate speed was 5 rad / min. Ar gas was continuously introduced during the sputtering process, and the deposition pressure was maintained at 1.2×10 -3 Pa, and a bias voltage of -65 V was applied to the substrate. The sputtering rates of Zr and Mo were 0.2 nm / s and 0.32 nm, respectively. The deposition time of Zr and Mo was set to 25 s, and the total thickness of the Zr / Mo metal multilayer film was 1.5 μm.

[0045] Step 4: The multilayer film obtained in step 3 is naturally cooled to room temperature in a high vacuum coating chamber and then taken out to obtain a Zr / Mo metal multilayer film with a single layer thickness of h=5 nm.

[0046] The microstructure of the prepared Zr / Mo metal multilayer film was characterized. The grains showed nano-columnar shape. The preferred orientation of the Mo layer was Mo (111) / / Si (100). The Zr layer had two preferred orientations: Zr (0002) / / Si (100) and Zr A semi-coherent interface is formed between Si (100), Zr, and Mo. Zr and Mo atomic layers alternate, with minimal intermixing between the atoms, resulting in a clear, flat interface. Nanoindentation testing reveals a hardness of 9.97 ± 0.32 GPa under a load of 5000 μN.

[0047] Example 2

[0048] A method for preparing a Zr / Mo metal multilayer film comprises the following steps:

[0049] Step 1: Take a single-side polished single-crystal Si substrate, ultrasonically clean it in chemically pure acetone and ethanol for 10 minutes, and then quickly dry it with warm air.

[0050] Step 2: Fix the single crystal silicon substrate after ultrasonic cleaning to the base plate and evacuate until the back vacuum is less than 5×10 -4 Pa.

[0051] Step 3: After the substrate is cleaned by ion bombardment using a small current, a direct current power supply is applied to the Zr target and the Mo target separately to alternately deposit a Zr / Mo metal multilayer film on the substrate.

[0052] The purity of the Zr target was 99.99 wt%, the DC power supply current was 2.4 A, the purity of the Mo target was 99.99 wt%, the DC power supply current was 2.4 A, and the substrate speed was 5 rad / min. Ar gas was continuously introduced during the sputtering process, and the deposition pressure was maintained at 1.2×10 -3 Pa, and a bias voltage of -65 V was applied to the substrate. The sputtering rates of Zr and Mo were 0.2 nm / s and 0.32 nm, respectively. The deposition time of Zr and Mo was set to 50 s, and the total thickness of the Zr / Mo metal multilayer film was 1.5 μm.

[0053] Step 4: The multilayer film obtained in step 3 is naturally cooled to room temperature in a high vacuum coating chamber and then taken out to obtain a Zr / Mo metal multilayer film with a single layer thickness of h=10 nm.

[0054] The microstructure of the prepared Zr / Mo metal multilayer film was characterized. The grains showed nano-columnar shape. The preferred orientation of the Mo layer was Mo (111) / / Si (100). The Zr layer had two preferred orientations: Zr (0002) / / Si (100) and Zr A semi-coherent interface is formed between Si (100), Zr, and Mo. Zr and Mo atomic layers alternate, with minimal intermixing between the atoms, resulting in a clear, straight interface. Nanoindentation testing reveals a hardness of 10.79 ± 0.29 GPa under a load of 5000 μN.

[0055] Example 3

[0056] A method for preparing a Zr / Mo metal multilayer film comprises the following steps:

[0057] Step 1: Take a single-side polished single-crystal Si substrate, ultrasonically clean it in chemically pure acetone and ethanol for 10 minutes, and then quickly dry it with warm air.

[0058] Step 2: Fix the single crystal silicon substrate after ultrasonic cleaning to the base plate and evacuate until the back vacuum is less than 5×10 -4 Pa.

[0059] Step 3: After the substrate is cleaned by ion bombardment using a small current, a direct current power supply is applied to the Zr target and the Mo target separately to alternately deposit a Zr / Mo metal multilayer film on the substrate.

[0060] The purity of the Zr target was 99.99 wt%, the DC power supply current was 2.4 A, the purity of the Mo target was 99.99 wt%, the DC power supply current was 2.4 A, and the substrate speed was 5 rad / min. Ar gas was continuously introduced during the sputtering process, and the deposition pressure was maintained at 1.2×10 -3Pa, and a bias voltage of -65 V was applied to the substrate. The sputtering rates of Zr and Mo were 0.2 nm / s and 0.32 nm, respectively. The deposition time of Zr and Mo was set to 100 s, and the total thickness of the Zr / Mo metal multilayer film was 1.5 μm.

[0061] Step 4: The multilayer film obtained in step 3 is naturally cooled to room temperature in a high vacuum coating chamber and then taken out to obtain a Zr / Mo metal multilayer film with a single layer thickness of h=20 nm.

[0062] The microstructure of the prepared Zr / Mo metal multilayer film was characterized. The grains showed nano-columnar shape. The preferred orientation of the Mo layer was Mo (111) / / Si (100). The Zr layer had two preferred orientations: Zr (0002) / / Si (100) and Zr A semi-coherent interface is formed between Si (100), Zr, and Mo. Zr and Mo atomic layers alternate, with minimal intermixing between the atoms, resulting in a clear, straight interface. Nanoindentation testing reveals a hardness of 9.91 ± 0.19 GPa under a load of 5000 μN.

[0063] Example 4

[0064] A method for preparing a Zr / Mo metal multilayer film comprises the following steps:

[0065] Step 1: Take a single-side polished single-crystal Si substrate, ultrasonically clean it in chemically pure acetone and ethanol for 10 minutes, and then quickly dry it with warm air.

[0066] Step 2: Fix the single crystal silicon substrate after ultrasonic cleaning to the base plate and evacuate until the back vacuum is less than 5×10 -4 Pa.

[0067] Step 3: After the substrate is cleaned by ion bombardment using a small current, a direct current power supply is applied to the Zr target and the Mo target separately to alternately deposit a Zr / Mo metal multilayer film on the substrate.

[0068] The purity of the Zr target was 99.99 wt%, the DC power supply current was 2.4 A, the purity of the Mo target was 99.99 wt%, the DC power supply current was 2.4 A, and the substrate speed was 5 rad / min. Ar gas was continuously introduced during the sputtering process, and the deposition pressure was maintained at 1.2×10 - 3 Pa, and a bias voltage of -65 V was applied to the substrate. The sputtering rates of Zr and Mo were 0.2 nm / s and 0.32 nm, respectively. The deposition time of Zr and Mo was set to 250 s, and the total thickness of the Zr / Mo metal multilayer film was 1.5 μm.

[0069] Step 4: The multilayer film obtained in step 3 is naturally cooled to room temperature in a high vacuum coating chamber and then taken out to obtain a Zr / Mo metal multilayer film with a single layer thickness of h=50nm.

[0070] The microstructure of the prepared Zr / Mo metal multilayer film was characterized. The grains showed nano-columnar shape. The preferred orientation of the Mo layer was Mo (111) / / Si (100). The Zr layer had two preferred orientations: Zr (0002) / / Si (100) and Zr A semi-coherent interface is formed between Si (100), Zr, and Mo. Zr and Mo atomic layers alternate, with minimal intermixing between the atoms, resulting in a clear, straight interface. Nanoindentation testing reveals a hardness of 10.40 ± 0.24 GPa under a load of 5000 μN.

[0071] Example 5

[0072] A method for preparing a Zr / Mo metal multilayer film comprises the following steps:

[0073] Step 1: Take a single-side polished single-crystal Si substrate, ultrasonically clean it in chemically pure acetone and ethanol for 10 minutes, and then quickly dry it with warm air.

[0074] Step 2: Fix the single crystal silicon substrate after ultrasonic cleaning to the base plate and evacuate until the back vacuum is less than 5×10 -4 Pa.

[0075] Step 3: After the substrate is cleaned by ion bombardment using a small current, a direct current power supply is applied to the Zr target and the Mo target separately to alternately deposit a Zr / Mo metal multilayer film on the substrate.

[0076] The purity of the Zr target was 99.99 wt%, the DC power supply current was 2.4 A, the purity of the Mo target was 99.99 wt%, the DC power supply current was 2.4 A, and the substrate speed was 5 rad / min. Ar gas was continuously introduced during the sputtering process, and the deposition pressure was maintained at 1.2×10 - 3 Pa, and a bias voltage of -65 V was applied to the substrate. The sputtering rates of Zr and Mo were 0.2 nm / s and 0.32 nm, respectively. The deposition time of Zr and Mo was set to 500 s, and the total thickness of the Zr / Mo metal multilayer film was 1.5 μm.

[0077] Step 4: The multilayer film obtained in step 3 is naturally cooled to room temperature in a high vacuum coating chamber and then taken out to obtain a Zr / Mo metal multilayer film with a single layer thickness of h=100 nm.

[0078] The microstructure of the prepared Zr / Mo metal multilayer film was characterized. The grains showed nano-columnar shape. The preferred orientation of the Mo layer was Mo (111) / / Si (100). The Zr layer had two preferred orientations: Zr (0002) / / Si (100) and Zr A semi-coherent interface is formed between Si (100), Zr, and Mo. Zr and Mo atomic layers alternate, with minimal intermixing between the atoms, resulting in a clear, straight interface. Nanoindentation testing reveals a hardness of 11.44 ± 0.08 GPa under a load of 5000 μN.

[0079] Example 6

[0080] A method for preparing a Zr / Mo metal multilayer film comprises the following steps:

[0081] Step 1: Take a single-side polished single-crystal Si substrate, ultrasonically clean it in chemically pure acetone and ethanol for 10 minutes, and then quickly dry it with warm air.

[0082] Step 2: Fix the single crystal silicon substrate after ultrasonic cleaning to the base plate and evacuate until the back vacuum is less than 5×10 -4 Pa.

[0083] Step 3: After the substrate is cleaned by ion bombardment using a small current, a direct current power supply is applied to the Zr target and the Mo target separately to alternately deposit a Zr / Mo metal multilayer film on the substrate.

[0084] The purity of the Zr target was 99.99 wt%, the DC power supply current was 2.4 A, the purity of the Mo target was 99.99 wt%, the DC power supply current was 2.4 A, and the substrate speed was 5 rad / min. Ar gas was continuously introduced during the sputtering process, and the deposition pressure was maintained at 1.2×10 - 3 Pa, and a bias voltage of -65 V was applied to the substrate. The sputtering rates of Zr and Mo were 0.2 nm / s and 0.32 nm, respectively. The deposition time of Zr and Mo was set to 750 s, and the total thickness of the Zr / Mo metal multilayer film was 1.5 μm.

[0085] Step 4: The multilayer film obtained in step 3 is naturally cooled to room temperature in a high vacuum coating chamber and then taken out to obtain a Zr / Mo metal multilayer film with a single layer thickness of h=150nm.

[0086] Microstructural characterization of the prepared Zr / Mo metallic multilayer film revealed nanocolumnar grains. The Mo layer exhibited a preferred orientation of Mo (111) / / Si (100), while the Zr layer exhibited two preferred orientations, similar to those described above. A semi-coherent interface was formed between Zr and Mo. The Zr and Mo atomic layers alternated with each other, with minimal intermixing between the atoms, resulting in a clear and flat interface. Nanoindentation testing revealed a hardness of 12.21±0.32 GPa under a load of 5000 μN.

[0087] Obviously, those skilled in the art may make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if such changes and modifications fall within the scope of the claims and their equivalents, the present invention is intended to include such changes and modifications.

Claims

1. A Zr / Mo metal multilayer film, characterized in that: The Zr / Mo metal multilayer film is a multilayer film with preferred orientation, including two different types of preferred orientations, namely Zr (0002) / / Mo (110) and Zr / / Mo (110); the multilayer film includes a Zr atomic layer and a Mo atomic layer, and the crystal grains in the Zr atomic layer and the Mo atomic layer are columnar nanocrystals; The Zr atomic layer and the Mo atomic layer are alternately distributed, and a Zr target and a Mo target are separately applied with a DC power supply to realize alternating deposition by a magnetron sputtering alternating deposition method. The sputtering rates of Zr and Mo are 0.2 nm / s and 0.32 nm / s, respectively. Ar gas is continuously introduced into the sputtering process of the magnetron sputtering alternating deposition, and the deposition gas pressure is maintained at During the deposition process, a bias voltage of -65V is applied to the substrate, and the thickness of the single layer in the Zr / Mo metal multilayer film is adjusted by changing the sputtering time. The total thickness of the Zr / Mo metal multilayer film is 1.5μm. During the sputtering process, the substrate temperature increases with the extension of the sputtering time and does not exceed 100°C. There is intermixing between the Zr atomic layer and the Mo atomic layer, and the layer thicknesses of the Zr atomic layer and the Mo atomic layer are equal.

2. The Zr / Mo metal multilayer film according to claim 1, wherein: The thickness of the Zr atomic layer and the Mo atomic layer are both 5-150 nm.

3. The Zr / Mo metal multilayer film according to claim 1, wherein: The nanoindentation hardness of the Zr / Mo metal multilayer film is in the range of 9.9-12.2 GPa, and when the layer thickness h>20 nm, the hardness decreases as the layer thickness decreases.

4. A method for preparing a Zr / Mo metal multilayer film, characterized in that: The method for preparing the Zr / Mo metal multilayer film according to any one of claims 1 to 3 comprises the following steps: Step 1: Clean and dry the surface of the single crystal Si substrate; Step 2: Place the substrate into the magnetron sputtering coating chamber and then evacuate it; Step 3: After the substrate is cleaned by ion bombardment, Zr / Mo metal multilayer films are alternately deposited on the substrate by magnetron sputtering; Step 4: The substrate obtained in step 3 is vacuum cooled, and the sputtered sample is taken out when the chamber temperature drops below 50°C.

5. The method for preparing a Zr / Mo metal multilayer film according to claim 4, wherein: The specific steps of cleaning and drying in step 1 are: The single crystal Si wafer was ultrasonically cleaned in acetone and alcohol for 10 minutes, and then dried. The roughness of the polished surface was less than 0.8 nm.

6. The method for preparing a Zr / Mo metal multilayer film according to claim 4, wherein: The vacuum degree of the vacuum pumping in step 2 is less than 5×10 -4 Pa.

7. The method for preparing a Zr / Mo metal multilayer film according to claim 4, wherein: The purity of the Zr target is 99.99 wt%, the DC power supply current is 2.4 A, the purity of the Mo target is 99.99 wt%, the DC power supply current is 2.4 A, and the base disk rotation speed is 5 rad / min.

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