Molybdenum disulfide / tungsten diboride nanocomposite multilayer film, and preparation method and application thereof

Abstract

The application provides a molybdenum disulfide tungsten diboride nanocomposite multilayer film and a preparation method and application thereof, and the molybdenum disulfide / tungsten diboride nanocomposite multilayer film is prepared by using a non-equilibrium magnetron sputtering technology, and comprises a titanium transition layer, a titanium / molybdenum disulfide / tungsten diboride multilayer gradient transition layer and a molybdenum disulfide / tungsten diboride multilayer doped layer which are sequentially stacked in the thickness direction, so as to obtain the molybdenum disulfide / tungsten diboride nanocomposite multilayer film. The molybdenum disulfide / tungsten diboride nanocomposite multilayer film has good substrate bonding strength, hardness and high hardness / elasticity ratio, the main phase molybdenum disulfide grows along the (002) crystal plane parallel to the substrate, the moisture resistance and high-temperature oxidation resistance of the molybdenum disulfide are greatly improved, the molybdenum disulfide exhibits excellent friction and wear performance under atmospheric normal temperature and high-temperature environment, and can meet the requirements of stable lubricating performance and long service life of key components of aerospace and nuclear energy machinery under harsh environment.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of surface protection, in particular to a molybdenum disulfide / molybdenum diboride nanocomposite multilayer film and a preparation method and application thereof. BACKGROUND

[0002] Molybdenum disulfide (MoS2) film has been widely used in aerospace, nuclear power, mechanical and electronic fields as a solid lubricant due to its unique structural characteristics and easy interlayer sliding. However, MoS2 is extremely sensitive to the environment and is easily oxidized in the atmosphere and at high temperatures, which leads to the decline of its tribological properties and the significant reduction of its service life. Spacecraft and satellite mechanical movement devices inevitably experience complex and harsh environmental conditions such as high humidity and high-low temperature alternation during transportation, storage and launching, which puts higher requirements on the reliability and stability of MoS2 film. In addition, the hardness of MoS2 film is relatively low, and it is prone to peeling and early failure under high-speed and heavy-load conditions. Therefore, it is urgent to develop a new MoS2-based nanometer lubricating film which integrates strength, toughness, corrosion resistance and low friction in a wide temperature range to ensure the long-life reliable service of key transmission components of high-tech equipment.

[0003] In recent years, borides have attracted much attention due to their high hardness, high melting point, high electrical conductivity and high thermal stability. Molybdenum diboride (WB2) has good high-temperature oxidation resistance and wear resistance, and as a doped phase, it can significantly improve the hardness and load capacity of MoS2 film, and improve the friction and wear properties of MoS2 film at high temperatures. The construction of the hetero-interface helps MoS2 grow along the (002) crystal plane parallel to the substrate to form a nanocomposite multilayer structure film with MoS2(002) / molybdenum diboride alternately grown, realizing the environmental self-adaptation and high-temperature low-friction wear of MoS2-based film. Chinese invention patent CN111621745A discloses a molybdenum disulfide / molybdenum disulfide multilayer tantalum-doped film and a preparation method and application thereof. In the method, a titanium transition layer, a titanium / tantalum / molybdenum disulfide / molybdenum disulfide multilayer gradient transition layer and a molybdenum disulfide / molybdenum disulfide multilayer tantalum-doped layer are sequentially deposited on the surface of the substrate by using a magnetron sputtering technology to obtain the molybdenum disulfide / molybdenum disulfide multilayer tantalum-doped film. The film is prepared by using the magnetron sputtering technology, and tantalum is doped in the molybdenum disulfide / molybdenum disulfide multilayer film to improve the mechanical properties and corrosion resistance of the film. However, the main body material of the film prepared by using the magnetron sputtering technology is MoS2 and WS2, and the mechanical properties of the film are relatively weak. In particular, the film prepared by using the patent needs to use expensive tantalum, which greatly increases the cost of raw materials.

[0004] Therefore, based on the problems of the prior art, the prepared molybdenum disulfide / tungsten diboride nanocomposite multilayer film does not need to be doped with noble metals, on the one hand, the raw material cost can be greatly reduced, on the other hand, by using the non-equilibrium magnetron sputtering technology, the nanometer gradient transition layer and the nanometer composite alternating multilayer are formed, the mutual diffusion and fusion between the interfaces are realized, the bonding force of the interfaces is enhanced, the mechanical properties and the tribological properties of the film are improved, the high-temperature friction performance is significantly improved, the raw material price is suitable, and the production cost is greatly reduced. SUMMARY

[0005] In view of the technical problems of the prior art, the application discloses a molybdenum disulfide / tungsten diboride nanocomposite multilayer film, a preparation method and application thereof.

[0006] To achieve the above-mentioned purpose, the application provides the following technical scheme, a molybdenum disulfide / tungsten diboride nanocomposite multilayer film, a titanium transition layer, a titanium / molybdenum disulfide / tungsten diboride gradient transition layer and a molybdenum disulfide / tungsten diboride nanocomposite multilayer film are sequentially deposited in the thickness direction of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film.

[0007] Preferably, the preparation method of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film comprises the following steps: a titanium transition layer, a titanium / molybdenum disulfide / tungsten diboride gradient transition layer and a molybdenum disulfide / tungsten diboride nanocomposite multilayer film are sequentially deposited on the surface of a substrate by using a non-equilibrium magnetron sputtering technology, so as to obtain the molybdenum disulfide / tungsten diboride nanocomposite multilayer film.

[0008] To achieve another purpose, the application further provides the preparation method of the above-mentioned molybdenum disulfide / tungsten diboride nanocomposite multilayer film, which comprises the following steps: a titanium transition layer, a titanium / molybdenum disulfide / tungsten diboride gradient transition layer and a molybdenum disulfide / tungsten diboride nanocomposite multilayer film are sequentially deposited on the surface of a substrate by using a non-equilibrium magnetron sputtering technology, so as to obtain the molybdenum disulfide / tungsten diboride nanocomposite multilayer film.

[0009] In some preferred embodiments, the preparation method comprises the following steps: a titanium metal target is used as a cathode target material, argon gas is used as a working gas, a target current is applied to the titanium metal target, a negative bias voltage is applied to the substrate, and then a titanium transition layer is deposited on the surface of the substrate by using a non-equilibrium magnetron sputtering technology.

[0010] In some preferred embodiments, the preparation method comprises the following steps: a titanium metal target, a molybdenum disulfide target and a tungsten diboride target are used as cathode target materials, argon gas is used as a working gas, target currents are applied to the titanium target, the molybdenum disulfide target and the tungsten diboride target, a negative bias voltage is applied to the substrate, and then a titanium / molybdenum disulfide / tungsten diboride gradient transition layer is deposited on the surface of the titanium transition layer by using a non-equilibrium magnetron sputtering technology.

[0011] In some preferred embodiments, the target current applied to the titanium target gradually decreases from the working current (3.0-5.0 A) to 0, and the target current of the molybdenum disulfide gradually increases from 0 to the working current 1.6 A; the target current applied to the tungsten diboride gradually increases from 0 to the working current 0.4-1.2 A, the substrate bias is -50--70 V, the working gas flow is 12-16 sccm, the cavity temperature is 80-120 ℃, the reaction chamber pressure is 0.1-0.4 Pa, and the deposition time is 1200-1800 s.

[0012] In some preferred embodiments, the thickness of the titanium / molybdenum disulfide / tungsten diboride gradient transition layer is 100-300 nm.

[0013] In some preferred embodiments, the preparation method comprises: using a non-equilibrium magnetron sputtering technology, using a molybdenum disulfide target and a tungsten diboride target as cathode target materials, using argon as a working gas, applying a target current to the molybdenum disulfide target and the tungsten diboride target, and applying a negative bias to the substrate, so as to grow a molybdenum disulfide / tungsten diboride nanocomposite multilayer film on the surface of the titanium / molybdenum disulfide / tungsten diboride gradient transition layer.

[0014] In some preferred embodiments, the target current applied to the molybdenum disulfide target is 1.6 A; the target current applied to the tungsten diboride target is 0.4 A or 0.6 A or 0.8 A or 1.0 A or 1.2 A, the substrate bias is -50--70 V, the control rotation speed of the turret is 2 revolutions, the working gas flow is 12-16 sccm, the substrate temperature is 80-120 ℃, the reaction chamber pressure is 0.1-0.4 Pa, and the deposition time is 6000-8000 s.

[0015] In some more preferred embodiments, the working current of the target current applied to the tungsten diboride is 0.6-1.2 A.

[0016] More preferably, the target current applied to the tungsten diboride is 1.0 A or 1.2 A.

[0017] Most preferably, the working current of the target current applied to the tungsten diboride is 1.0 A.

[0018] In some preferred embodiments, the preparation method comprises: using a non-equilibrium magnetron sputtering technology, applying a high target current to the tungsten diboride target, so as to realize the diffusion of the tungsten diboride to the molybdenum disulfide layer, obtain a strong-bonding molybdenum disulfide / tungsten diboride heterojunction interface, and be different from traditional composite and multilayer films.

[0019] The embodiments of the present application also provide a cross section of two films, comprising a substrate, and the aforementioned molybdenum disulfide / tungsten diboride nanocomposite multilayer film deposited on the substrate.

[0020] The molybdenum disulfide / tungsten diboride nanocomposite multilayer film is applied to the field of aerospace, nuclear energy mechanical movement device surface protection.

[0021] In some preferred embodiments, the application relates to a device comprising a substrate, wherein the substrate is further provided with the aforementioned molybdenum disulfide / tungsten diboride nanocomposite multilayer film.

[0022] Further, the substrate material is not limited, and can be a single crystal silicon wafer, and / or 316 stainless steel, and / or 9Cr18, and / or T6AL4V, etc., but is not limited thereto.

[0023] Further, the device further comprises an aerospace vehicle and a nuclear power bearing, but is not limited thereto.

[0024] In order to further illustrate the technical effects of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared by the above technical solution, the following will make a detailed comparison with the prior art:

[0025] The hardness of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film obtained by the best embodiment of the application is 8.03 GPa, and the hardness / elasticity is as high as 0.098, close to 0.1, indicating excellent mechanical properties and wear resistance. The main body material of the film prepared by the prior art (see CN111621745A) is MoS2 and WS2, and the mechanical properties of the film are relatively weak. The hardness of the best embodiment is only 7.4 GPa, and the hardness / elasticity ratio is 0.083; the high-temperature wear rate is in the order of 10 -6 mm 3 / N·m; compared with the prior art, the non-equilibrium magnetron sputtering technology used in the application can improve the mechanical properties of the film, especially the high-temperature wear rate is in the order of 10 -7 mm 3 / N·m, which is reduced by one order of magnitude.

[0026] Further, in terms of structure, the molybdenum disulfide / tungsten disulfide in the prior art is still a traditional multilayer structure, the thickness of the molybdenum disulfide layer or the tungsten disulfide layer in one modulation period is greater than 10 nm, and the layer-to-layer interface is clear. Such a multilayer structure with a clear interface structure is extremely prone to peeling of the thin film under force due to the mechanical property difference between different materials. The nano-composite multilayer structure prepared by the technical scheme of the present application has a total thickness of the molybdenum disulfide / tungsten disulfide in one modulation period less than 10 nm, and the non-equilibrium magnetron sputtering technology adopted in the present application causes the mutual diffusion between the molybdenum disulfide and the tungsten disulfide with a nanometer size effect, promotes the mutual fusion of the interfaces between the molybdenum disulfide layer and the tungsten disulfide layer, and thus the interface bonding of the obtained thin film is good, and the mechanical property and the tribological property of the thin film are improved, and the peeling of the thin film under force is avoided.

[0027] The present application has at least the following beneficial effects:

[0028] (1) The molybdenum disulfide / tungsten disulfide nano-composite multilayer thin film provided by the technical scheme of the present application has good film-to-substrate bonding strength, high hardness and high hardness / elasticity ratio due to the design of the doped tungsten disulfide hard ceramic phase and the gradient transition layer.

[0029] (2) The molybdenum disulfide / tungsten disulfide nano-composite multilayer thin film provided by the technical scheme of the present application has low friction coefficient and wear rate under atmospheric (50±5% humidity) normal temperature and high temperature (100℃, 200℃, 300℃) conditions due to the combination of the doped tungsten disulfide hard ceramic phase and the gradient transition layer, the good self-lubricating property of the molybdenum disulfide and the excellent wear resistance of the tungsten disulfide, and thus the environmental self-adaptation and high-temperature oxidation resistance of the molybdenum disulfide-based thin film are realized. Therefore, the molybdenum disulfide / tungsten disulfide nano-composite multilayer thin film can meet the long-life reliable service of aerospace vehicles and nuclear power bearings under harsh environments.

[0030] (3) Compared with the preparation method of the prior art, the technical scheme of the present application does not need to dope noble metals such as tantalum, reduces the cost, and has the advantages of simple operation and easy control, and is very suitable for popularization and promotion of industrial production. BRIEF DESCRIPTION OF DRAWINGS

[0031] Figure 1 is the XRD pattern of the molybdenum disulfide / tungsten disulfide nano-composite multilayer thin film prepared by the examples 1-5 of the present application and the pure molybdenum disulfide thin film prepared by the comparative example 1.

[0032] Figure 2a is the cross-sectional SEM pattern of the molybdenum disulfide / tungsten disulfide nano-composite multilayer thin film prepared by the example 1 of the present application.

[0033] Figure 2bis a cross-sectional SEM image of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared in Example 4 of the present application.

[0034] Figure 3a is a cross-sectional TEM image of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared in Example 1 of the present application.

[0035] Figure 3b is a cross-sectional TEM image of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared in Example 4 of the present application.

[0036] Figure 4a is a high-resolution TEM image of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared in Example 1 of the present application.

[0037] Figure 4b is a high-resolution TEM image of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared in Example 4 of the present application.

[0038] Figure 5 is a graph of the friction coefficient curve of the molybdenum disulfide / tungsten diboride nanocomposite multilayer films prepared in Examples 1-5 of the present application and the pure molybdenum disulfide film prepared in Comparative Example 1 under atmospheric temperature environment.

[0039] Figure 6 is a graph of the average friction coefficient and the wear rate of the molybdenum disulfide / tungsten diboride nanocomposite multilayer films prepared in Examples 1-5 of the present application and the pure molybdenum disulfide film prepared in Comparative Example 1 under atmospheric temperature environment.

[0040] Figure 7 is a graph of the friction coefficient curve of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared in Example 4 of the present application and the pure molybdenum disulfide film prepared in Comparative Example 1 at 100°C.

[0041] Figure 8 is a graph of the friction coefficient curve of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared in Example 4 of the present application and the pure molybdenum disulfide film prepared in Comparative Example 1 at 200°C.

[0042] Figure 9 is a graph of the friction coefficient curve of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared in Example 4 of the present application and the pure molybdenum disulfide film prepared in Comparative Example 1 at 300°C.

[0043] Figure 10 is a graph of the average friction coefficient of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared in Example 4 of the present application and the pure molybdenum disulfide film prepared in Comparative Example 1 under atmospheric high temperature environment (100-300°C).

[0044] Figure 11is a wear rate graph of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared in Example 4 of the present invention and the pure molybdenum disulfide film prepared in Comparative Example 1 in an atmospheric high-temperature environment (100-300°C). DETAILED DESCRIPTION

[0045] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described. Obviously, the described embodiments are only some of the embodiments of the present application, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort belong to the protection scope of the present invention.

[0046] The disclosures of all patent and non-patent literature cited in the present invention are incorporated herein by reference in their entirety.

[0047] As used in the present invention, the terms "comprise", "include", "contain", "cover", "have", "possess", or any other variant thereof are intended to cover non-exclusive inclusion. For example, a process, method, article, or device including a list of elements does not necessarily limit to those elements only, but can include other elements not explicitly listed or inherent to such process, method, article, or device. In addition, unless explicitly indicated to the contrary, "or" refers to inclusive "or" rather than exclusive "or".

[0048] In addition, "one" or "an" is used to describe elements and components of the present invention. This is done only for convenience and to provide a general sense of the scope of the invention. This description should be understood to include one or at least one and the singular also includes the plural, unless it is explicitly stated otherwise.

[0049] Some embodiments of the present invention provide a molybdenum disulfide / tungsten diboride nanocomposite multilayer film, which comprises a titanium transition layer, a titanium / molybdenum disulfide / tungsten diboride gradient transition layer, and a molybdenum disulfide / tungsten diboride nanocomposite multilayer deposited in the order in the thickness direction of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film.

[0050] Further, the thickness of the titanium transition layer is controlled to be 100-300 nm.

[0051] Further, the thickness of the titanium / molybdenum disulfide / tungsten diboride gradient transition layer is controlled to be 200-400 nm.

[0052] Further, the thickness of the molybdenum disulfide / tungsten diboride nanocomposite multilayer is 2.1 μm-2.8 μm.

[0053] Further, the hardness of the MoS2 / WB2 nanocomposite multilayer film is up to 9.54 GPa, and the ratio of hardness to elasticity is up to 0.098.

[0054] Further, the friction coefficient of the MoS2 / WB2 nanocomposite multilayer film at room temperature in air is 0.05-0.15, and the wear rate is 1.88*10 -7 -1.58*10 -6 mm 3 / N·m.

[0055] Further, the friction coefficient of the MoS2 / WB2 nanocomposite multilayer film at 100℃ is 0.02-0.16, and the wear rate is 3.62*10 -7 -1.09*10 -6 mm 3 / N·m; the friction coefficient at 200℃ is 0.04-0.20, and the wear rate is 3.96*10 -7 -1.70*10 -6 mm 3 / N·m; the friction coefficient at 300℃ is 0.07-0.50, and the wear rate is 9.30*10 -7 -1.27*10 -5 mm 3 / N·m.

[0056] As another aspect of the technical scheme of the present application, the preparation method of the aforementioned MoS2 / WB2 nanocomposite multilayer film comprises: sequentially depositing a titanium transition layer, a titanium / MoS2 / WB2 gradient transition layer and a MoS2 / WB2 nanocomposite multilayer film on the surface of a substrate by using a non-equilibrium magnetron sputtering technology.

[0057] In some embodiments, the method for preparing the titanium transition layer comprises: using a titanium target as a cathode target material, using argon as a working gas, applying a target current to the titanium target, applying a negative bias to the substrate, and thereby depositing a titanium transition layer on the surface of the substrate by using a non-equilibrium magnetron sputtering technology, wherein the target current is 3.0-5.0 A, the substrate bias is -70 to -90 V, the working gas flow rate is 12-16 sccm, the substrate temperature is 80-120℃, and the reaction chamber pressure is 0.1-0.4 Pa.

[0058] Further, the working gas is an inert gas, preferably argon, but not limited thereto.

[0059] Further, the thickness of the titanium transition layer is about 100-300 nm.

[0060] In some embodiments, the method for preparing the gradient transition layer comprises: using a non-equilibrium magnetron sputtering technique, taking a titanium target, a molybdenum disulfide target, and a tungsten diboride target as cathode target materials, taking argon as a working gas, applying a target current to the titanium target, the molybdenum disulfide target, and the tungsten diboride target, and applying a negative bias to the substrate, so as to deposit a titanium / molybdenum disulfide / tungsten diboride gradient transition layer on the surface of the titanium transition layer, wherein the target current applied to the titanium target is gradually reduced from a working current (3.0-5.0 A) to 0, the target current of the molybdenum disulfide is gradually increased from 0 to a working current (1.6 A), the target current applied to the tungsten diboride is gradually increased from 0 to a working current (0.4 A, or 0.6 A, or 0.8 A, or 1.0 A, or 1.2 A), the substrate bias is -50 to -70 V, the working gas flow is 12-16 sccm, the cavity temperature is 80-120°C, the reaction chamber pressure is 0.1-0.4 Pa, and the deposition time is 1200-1800 s; preferably, the thickness of the titanium / molybdenum disulfide / tungsten diboride gradient transition layer is between 100-300 nm.

[0061] Further, the working gas is an inert gas, preferably argon, but is not limited thereto.

[0062] Further, the thickness of the titanium / molybdenum disulfide / tungsten diboride gradient transition layer is about 200-400 nm.

[0063] In some embodiments, the method for preparing the gradient transition layer comprises: using a non-equilibrium magnetron sputtering technique, taking a titanium target, a molybdenum disulfide target, and a tungsten diboride target as cathode target materials, taking argon as a working gas, applying a target current to the titanium target, the molybdenum disulfide target, and the tungsten diboride target, and applying a negative bias to the substrate, so as to deposit a titanium / molybdenum disulfide / tungsten diboride gradient transition layer on the surface of the titanium transition layer, wherein the target current applied to the titanium target is gradually reduced from a working current (3.0-5.0 A) to 0, the target current of the molybdenum disulfide is gradually increased from 0 to a working current (1.6 A), the target current applied to the tungsten diboride is gradually increased from 0 to a working current (0.4 A, or 0.6 A, or 0.8 A, or 1.0 A, or 1.2 A), the substrate bias is -50 to -70 V, the working gas flow is 12-16 sccm, the cavity temperature is 80-120°C, the reaction chamber pressure is 0.1-0.4 Pa, and the deposition time is 1200-1800 s; preferably, the thickness of the titanium / molybdenum disulfide / tungsten diboride gradient transition layer is between 100-300 nm.

[0064] Further, the working gas is an inert gas, preferably argon, but is not limited thereto.

[0065] Further, the thickness of the titanium / molybdenum disulfide / tungsten diboride gradient transition layer is about 200-400 nm.

[0066] In some more specific embodiments, the method for preparing the molybdenum disulfide / tungsten diboride nanocomposite multilayer film comprises the following steps:

[0067] (1) the titanium target current is 5.0 A, the substrate bias is -70 to -90 V, the working gas is argon, the gas flow is 12 to 16 sccm, the deposition substrate temperature is 80 to 120 °C, the pressure is 0.1 to 0.4 Pa, and the deposition time is 1200 to 1800 s, and a titanium transition layer is deposited on the surface of the substrate;

[0068] (2) the titanium target current gradually decreases from 5.0 A to 0, the target current of the molybdenum disulfide target gradually increases to 1.6 A, the target current applied to the tungsten diboride target gradually increases to 0.4 to 1.2 A, the substrate bias is -50 to -70 V, the working gas flow is 12 to 16 sccm, the substrate temperature is 80 to 120 °C, the reaction chamber pressure is 0.1 to 0.4 Pa, and the deposition time is 1200 to 1800 s, and then a titanium / molybdenum disulfide / tungsten diboride gradient transition layer is deposited on the surface of the titanium transition layer, and the thickness of the transition layer is controlled to be 200 to 400 nm;

[0069] (3) the molybdenum disulfide target sputtering current is kept at 1.6 A, and the tungsten diboride target sputtering current is 0.4 to 1.2 A until the molybdenum disulfide / tungsten diboride nanocomposite multilayer film reaches a thickness of 2.1 μm to 2.8 μm.

[0070] In some embodiments, the tungsten diboride target sputtering current is 0.4 A, 0.6 A, 0.8 A, 1.0 A, and 1.2 A, respectively, and when the current is 0.4 A, the MoS2 / WB2 nanocomposite multilayer film has a relatively insignificant MoS2(002) orientation growth preference, but as the current gradually increases, the growth preference becomes more obvious, and when the current is 1.0 A, the growth preference reaches an optimum.

[0071] In some embodiments, the preparation method further comprises: controlling the rotation speed of the sample holder to be within 2 revolutions per minute, thereby obtaining a molybdenum disulfide / tungsten diboride nanocomposite multilayer structure.

[0072] Further, the preparation method further comprises: after the reaction cavity is pumped to a predetermined vacuum degree (3×10 -3 Pa or less), the surface of the substrate is subjected to plasma etching treatment to remove the surface oxide of the substrate; and the specific etching method comprises applying a bias of -400 to -500 V to the substrate, the etching substrate temperature is 100 to 150 °C, and the etching time is 1200 to 1800 s.

[0073] Further, the substrate material is not limited, and can be a single crystal silicon wafer, and / or 316 stainless steel, and / or 9Gr18, and / or T6AL4V, etc., but is not limited thereto.

[0074] As another aspect of the technical solution of the present application, it relates to the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared by the method.

[0075] As another aspect of the technical solution of the present application, it relates to the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared by the method.

[0076] Further, the substrate material is not limited to monocrystalline silicon wafer, and / or 316 stainless steel, and / or 9Cr18, and / or T6AL4V, etc., but is not limited thereto.

[0077] As another aspect of the technical solution of the present application, it relates to a device comprising a substrate, wherein the substrate is further provided with the molybdenum disulfide / tungsten diboride nanocomposite multilayer film.

[0078] Further, the substrate material is not limited to monocrystalline silicon wafer, and / or 316 stainless steel, and / or 9Cr18, and / or T6AL4V, etc., but is not limited thereto.

[0079] Further, the device includes an aerospace vehicle and a nuclear power bearing, but is not limited thereto.

[0080] The present inventors also tested the molybdenum disulfide / tungsten diboride nanocomposite multilayer film prepared in the best embodiment as follows:

[0081] The hardness and elastic modulus of the film were measured by using MTS NanoIndenter G200 nanoindentation system, diamond indenter, and the indentation depth was less than 1 / 10 of the film thickness to avoid the influence of the substrate, and the average value of six points was measured. The test results show that the hardness of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film is greater than 7 GPa, and the hardness / elasticity ratio is greater than 0.09.

[0082] Friction and wear test, using Anton Paar friction and wear tester, under the condition of atmospheric humidity of 50±5%RH, test temperature of 25±3℃, the friction and wear performance of the film was analyzed. GCr15 steel ball was used as the friction pair, using reciprocating sliding mode, frequency of 5Hz, sliding step of 5mm, running time of 1h, normal load of 5N. At the same time, using Anton Paar multifunctional high temperature friction tester to analyze the high temperature friction and wear performance of the film, the test temperature was 100℃, 200℃, 300℃. GCr15 steel ball was used as the friction pair, using cyclic rotation mode, linear speed of 12.56cm / s, rotation radius of 4mm, running time of 1h, normal load of 5N. The cross section of the wear area was measured by using the contact type step meter, and the wear volume of the film was calculated by multiplying the sliding step, and the wear rate was obtained by dividing the wear volume by the load and the total sliding distance.

[0083] Test results: the film provided by the application has a friction coefficient of 0.056 and a wear rate of 1.88×10 - 7 mm 3 / N·m at 100℃, a friction coefficient of 0.019 and a wear rate of 3.62×10 -7 mm 3 / N·m at 200℃, a friction coefficient of 0.051 and a wear rate of 3.96×10 -7 mm 3 / N·m at 300℃, a friction coefficient of 0.070 and a wear rate of 9.30×10 -6 mm 3 / N·m.

[0084] In summary, by the above technical scheme, the molybdenum disulfide / tungsten diboride nano composite multilayer film provided by the application has good mechanical properties, exhibits low friction and wear performance in high temperature environment, and can meet the long life and reliable service of aerospace vehicles and nuclear power mechanical moving devices in harsh environment.

[0085] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs. Although methods and materials similar or equivalent to those described herein can be used in the practice or testing of embodiments of the disclosed compositions, suitable methods and materials are described below. All publications, patent applications, patents, and other references mentioned herein are incorporated by reference in their entirety unless a particular passage is cited. In case of conflict between the disclosure and the incorporated references, the disclosure will control. In addition, the materials, methods, and examples are illustrative only and not intended to be limiting.

[0086] The technical solutions of the present application, its implementation process and principles will be further explained and described through specific examples as follows. It should be pointed out that the following detailed description is exemplary and is intended to provide further description of the present application. The described examples are only a part of the examples of the present application, but not all. Based on the examples in the present application, all other examples obtained by those skilled in the art without creative labor fall within the scope of protection of the present application. Unless otherwise specified, the reagents and raw materials used in the following examples are commercially available, and the test methods not specified in the following examples are generally carried out under conventional conditions or under the conditions recommended by the manufacturers. In addition, unless otherwise specified, the experimental methods, detection methods, and preparation methods disclosed in the present application all use conventional techniques in the technical field. These techniques have been well described in existing literature.

[0087] Example 1

[0088] This example provides a MoS2 / WB2 nanocomposite multilayer film, wherein the base materials are 316 stainless steel and monocrystalline silicon wafer, respectively. Among them, after the deposition of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film on the 316 stainless steel base material, the service performance test can be carried out, including related mechanical properties, atmospheric room temperature friction performance test, etc.; after the deposition of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film on the monocrystalline silicon wafer base material, the thickness and structure of the film can be tested. The steps and methods of film deposition are the same for the two different base materials, and the difference in the base material itself has no effect on the physicochemical properties of the film. Other examples are the same.

[0089] In this example, a non-equilibrium magnetron sputtering technique is used to prepare a molybdenum disulfide / tungsten diboride nanocomposite multilayer film on the surface of the above-mentioned base, mainly including the following steps:

[0090] The mechanically polished base material is placed in an acetone solution for ultrasonic cleaning for 15 minutes and dried with nitrogen; then it is placed in an anhydrous ethanol solution for ultrasonic cleaning for 15 minutes and dried with nitrogen for standby use.

[0091] Arrange the target positions in a counterclockwise direction: two MoS2 targets (purity 99.9 at.%), one Ti target (purity 99.99 at.%), one MoS2 target (purity 99.9 at.%), one WB2 target (purity 99.99 at.%), and one MoS2 target (purity 99.99 at.%).

[0092] Place the cleaned base into a non-equilibrium magnetron sputtering chamber, and vacuumize to a vacuum degree lower than 3x10 -3Pa, the cavity is filled with high-purity argon gas, and then the target material is cleaned by argon plasma sputtering for 30 minutes, and the substrate temperature is 100-120°C. The non-equilibrium magnetron sputtering technology is used to prepare the MoS2 / WB2 nano-composite multilayer film, and the specific steps are as follows:

[0093] (1) Substrate surface treatment: a bias voltage of-500V is applied to the substrate, and the substrate surface is etched by plasma for 30 minutes, and the substrate temperature is about 100°C.

[0094] (2) Ti transition layer deposition: Ti target current is 3.0A, substrate bias is-70V, working gas is argon, gas flow is 16sccm, substrate deposition temperature is 80°C, pressure is about 0.2Pa, deposition time is 1200s, Ti transition layer is deposited on the substrate surface, thickness is about 200nm;

[0095] (3) Ti / MoS2 / WB2 gradient transition layer: Ti target current gradually decreases to 0A, while MoS2 target current gradually increases to 1.6A, and WB2 target current gradually increases to 0.4A, working gas is Ar, gas flow is 16sccm, substrate bias is-50V, substrate deposition temperature is about 100°C, pressure is about 0.2Pa, deposition time is 1800s, Ti / MoS2 / WB2 gradient transition layer is deposited on the surface of Ti transition layer, thickness is about 200nm;

[0096] (4) MoS2 / WB2 nano-composite multilayer: MoS2 target current is kept at 1.6A, WB2 target current is kept at 0.4A, and the rest of the deposition parameters remain unchanged, deposition time is 7000s; the thickness modulation ratio of MoS2 layer to WB2 layer is controlled to be 3-4:1; the thickness of MoS2 single layer is about 6nm, the thickness of WB2 single layer is about 1.5nm; the thickness of MoS2 / WB2 nano-composite multilayer is about 1.8μm; the total thickness of MoS2 / WB2 nano-composite multilayer film is controlled to be about 2.2μm.

[0097] The MoS2 / WB2 nano-composite multilayer film obtained by the above deposition is tested for structure, mechanical properties and friction and wear properties, which specifically includes:

[0098] (1) Structure test:

[0099] Referring to Figure 1 , the XRD test results of the MoS2 / WB2 nano-composite multilayer film prepared in this embodiment, the MoS2 / WB2 nano-composite multilayer film grows preferentially in the MoS2(002) orientation, which is not obvious.

[0100] Referring to Figure 2aThe SEM image of the cross section of the thin film prepared in the embodiment is shown in Figure 1. The thickness of the Ti transition layer is about 200 nm, the thickness of the Ti / MoS2 / WB2 nanometer gradient transition layer is about 200 nm, the thickness of the MoS2 / WB2 nanometer composite multilayer is about 1.8 μm, and the total thickness of the MoS2 / WB2 nanometer composite multilayer thin film is about 2.2 μm.

[0101] Referring to Figure 3a The cross-sectional TEM image of the MoS2 / WB2 nanometer composite multilayer thin film prepared in the embodiment is shown in Figure 2. Further, as shown in the figure, the interface between the layers in the figure is hardly visible, indicating that mutual diffusion occurs between MoS2 and WB2, enhancing the interface bonding force and avoiding the occurrence of peeling under stress, thereby providing a structural basis for improving tribological properties.

[0102] Referring to Figure 4a The high-resolution TEM image of the MoS2 / WB2 nanometer composite multilayer thin film prepared in the embodiment is shown in Figure 3. In the MoS2 / WB2 nanometer composite multilayer of the thin film, the thickness of the MoS2 layer is about 6 nm, the thickness of the WB2 layer is about 1.5 nm, and the thickness modulation ratio of the MoS2 layer and the WB2 layer is controlled at 4:1.

[0103] (2) Mechanical property test:

[0104] The hardness and elastic modulus of the thin film were measured by using the MTS NanoIndenter G200 nanoindentation system. The indentation depth of the diamond indenter was 1 / 10 of the film thickness, and the average value of six points was measured. The test results are shown in Table 1.

[0105] (3) Tribological property test:

[0106] The tribological property of the thin film was analyzed by using the Anton Paar multifunctional friction tester. The atmospheric humidity was 50±5% RH, the test temperature was 25±3°C, a GCr15 steel ball was used as the friction pair, a reciprocating sliding mode was used, the frequency was 5 Hz, the sliding step was 5 mm, the running time was 1 h, and the normal load was 5 N. The contact step meter was used to measure the wear volume, and the wear volume was divided by the load and the total sliding distance to obtain the wear rate. The test results of the atmospheric room temperature friction coefficient and the wear rate of the thin film are shown in Table 2. Figure 6

[0107] Example 2

[0108] ​In this embodiment, the base material is 316 stainless steel and single crystal silicon wafer. Among them, the 316 stainless steel is used as the base material for the deposition of molybdenum disulfide / tungsten diboride nano composite multilayer film, which can be used for service performance detection, including related mechanical properties, atmospheric room temperature friction performance test, etc.; the single crystal silicon wafer is used as the base material for the deposition of molybdenum disulfide / tungsten diboride nano composite multilayer film, which can be used for the test of film thickness, structure, etc.

[0109] The non-equilibrium magnetron sputtering technology is used to prepare the molybdenum disulfide / tungsten diboride nano composite multilayer film on the surface of the substrate, which mainly includes the following steps:

[0110] The mechanically polished base material is placed in an acetone solution for ultrasonic cleaning for 15 minutes and dried with nitrogen; then it is placed in an anhydrous ethanol solution for ultrasonic cleaning for 15 minutes and dried with nitrogen for standby.

[0111] The target position is arranged in a counterclockwise direction: two MoS2 targets (purity 99.9at.%), one Ti target (purity 99.99at.%), one MoS2 target (purity 99.9at.%), one WB2 target (purity 99.99at.%), and one MoS2 target (purity 99.99at.%).

[0112] The cleaned substrate is placed in a non-equilibrium magnetron sputtering chamber, and the vacuum degree is less than 3×10 -3 Pa, then high-purity argon gas is filled into the chamber, and then the target material is sputtered by argon plasma for 30 min, and the substrate temperature is 100-120°C. The non-equilibrium magnetron sputtering technology is used to prepare the MoS2 / WB2 nano composite multilayer film with a sample holder rotation speed of 2 revolutions per minute, and the specific steps are as follows:

[0113] (1) Substrate surface treatment: a bias voltage of -500V is applied to the substrate, and plasma etching is performed for 30 min, with a substrate temperature of about 100°C, to remove the surface oxide of the substrate.

[0114] (2) Ti transition layer deposition: Ti target current is 3.0A, substrate bias is -70V, working gas is argon, gas flow is 16sccm, substrate deposition temperature is 80°C, pressure is about 0.2Pa, deposition time is 1200s, Ti transition layer with a thickness of about 200nm is deposited on the substrate surface;

[0115] (3) Ti / MoS2 / WB2 gradient transition layer: gradually reduce the Ti target current to 0 A, while gradually increase the MoS2 target current to 1.6 A and the WB2 target current to 0.6 A, the working gas is Ar, the gas flow is 16 sccm, the substrate bias is -50 V, the substrate deposition temperature is about 100 ℃, the pressure is about 0.2 Pa, and the deposition time is 1800 s, to deposit a Ti / MoS2 / WB2 gradient transition layer with a thickness of about 200 nm on the surface of the Ti transition layer;

[0116] (4) MoS2 / WB2 nanocomposite multilayer: keep the MoS2 target current at 1.6 A and the WB2 target current at 0.6 A, and keep the rest of the deposition parameters unchanged, the deposition time is 7000 s, and the thickness modulation ratio of MoS2 layer to WB2 layer is controlled to be 3-4:1; wherein the thickness of a single MoS2 layer is about 6 nm, and the thickness of a single WB2 layer is about 1.6 nm; the thickness of the MoS2 / WB2 nanocomposite multilayer is about 1.8 μm; and the total thickness of the MoS2 / WB2 nanocomposite multilayer is controlled to be about 2.4 μm.

[0117] The MoS2 / WB2 nanocomposite multilayer film obtained by the above deposition is tested as follows:

[0118] (1) Structure test:

[0119] Referring to Figure 1 , the XRD test results of the MoS2 / WB2 nanocomposite multilayer film prepared in this embodiment, the MoS2 / WB2 nanocomposite multilayer film grows preferentially in the MoS2(002) orientation.

[0120] (2) Mechanical property test:

[0121] The hardness and elastic modulus of the film are measured by using the MTS NanoIndenter G200 nanoindentation instrument system, the indentation depth of the diamond indenter is 1 / 10 of the film thickness, six points are measured and averaged, and the test results are shown in Table 2.

[0122] (3) Friction and wear property test:

[0123] The Anton Paar multifunctional friction tester is used to analyze the tribological properties of the film, the atmospheric humidity is 50±5% RH, the test temperature is 25±3 ℃, the GCr15 steel ball is used as the friction pair, the reciprocating sliding mode is adopted, the frequency is 5 Hz, the sliding step is 5 mm, the running time is 1 h, and the normal load is 5 N. The contact type step meter is used to measure the wear volume, and the wear rate is obtained by dividing the wear volume by the load and the total sliding distance. The test results of the atmospheric room temperature environment friction coefficient and the wear rate of the film are shown in Figure 6 .

[0124] Example 3

[0125] In this embodiment, the base material is 316 stainless steel and single crystal silicon wafer. Among them, the 316 stainless steel is used as the base material for the deposition of molybdenum disulfide / tungsten diboride nano composite multilayer film, which can be used for service performance detection, including related mechanical properties, atmospheric room temperature friction performance test, etc. The single crystal silicon wafer is used as the base material for the deposition of molybdenum disulfide / tungsten diboride nano composite multilayer film, which can be used for the test of film thickness, structure, etc.

[0126] The non-equilibrium magnetron sputtering technology is used to prepare the molybdenum disulfide / tungsten diboride nano composite multilayer film on the surface of the base, which mainly includes the following steps:

[0127] The mechanically polished base material is placed in an acetone solution for ultrasonic cleaning for 15 minutes and dried with nitrogen; then it is placed in an anhydrous ethanol solution for ultrasonic cleaning for 15 minutes and dried with nitrogen for standby.

[0128] The target position is arranged in a counterclockwise direction: two MoS2 targets (purity 99.9at.%), one Ti target (purity 99.99at.%), one MoS2 target (purity 99.9at.%), one WB2 target (purity 99.99at.%), and one MoS2 target (purity 99.99at.%).

[0129] The cleaned base is placed in a non-equilibrium magnetron sputtering chamber, and the vacuum degree is reduced to less than 3×10 -3 Pa, then high-purity argon gas is filled into the chamber, and then the target material is sputtered by argon plasma for 30 min with a base temperature of 100-120°C. The non-equilibrium magnetron sputtering technology is used to prepare the MoS2 / WB2 nano composite multilayer film with a sample holder rotation speed of 2 revolutions per minute. The specific steps are as follows:

[0130] (1) Base surface treatment: a bias voltage of -500V is applied to the substrate, and plasma etching is used for 30 min with a base temperature of about 100°C to remove the surface oxide of the base.

[0131] (2) Ti transition layer deposition: the Ti target current is 3.0A, the base bias voltage is -70V, the working gas is argon, the gas flow is 16sccm, the base deposition temperature is 80°C, the pressure is about 0.2Pa, and the deposition time is 1200s. A Ti transition layer with a thickness of about 200nm is deposited on the surface of the base.

[0132] (3) Ti / MoS2 / WB2 gradient transition layer: the Ti target current is gradually reduced to 0 A, while the MoS2 target current is gradually increased to 1.6 A and the WB2 target current is gradually increased to 0.8 A, the working gas is Ar, the gas flow is 16 sccm, the substrate bias is -50 V, the substrate deposition temperature is about 100 ℃, the pressure is about 0.2 Pa, and the deposition time is 1800 s, and a Ti / MoS2 / WB2 gradient transition layer with a thickness of about 200 nm is deposited on the surface of the Ti transition layer;

[0133] (4) MoS2 / WB2 nanocomposite multilayer: the MoS2 target current is kept at 1.6 A and the WB2 target current is kept at 0.8 A, and the rest of the deposition parameters remain unchanged, the deposition time is 7000 s, and the thickness modulation ratio of the MoS2 layer to the WB2 layer is controlled to be 3-4:1; wherein the thickness of the MoS2 single layer is about 6 nm, the thickness of the WB2 single layer is about 1.8 nm, the thickness of the MoS2 / WB2 nanocomposite multilayer is about 1.8 μm, and the total thickness of the MoS2 / WB2 nanocomposite multilayer is controlled to be about 2.5 μm.

[0134] The MoS2 / WB2 nanocomposite multilayer film obtained by the above deposition is tested as follows:

[0135] (1) Structure test:

[0136] Referring to Figure 1 , the XRD test results of the MoS2 / WB2 nanocomposite multilayer film prepared in this embodiment, the MoS2 / WB2 nanocomposite multilayer film grows preferentially in the MoS2(002) orientation.

[0137] (2) Mechanical property test:

[0138] The hardness and elastic modulus of the film are measured by MTS NanoIndenter G200 nanoindentation instrument system, the indentation depth of the diamond indenter is 1 / 10 of the film thickness, six points are measured and averaged, and the test results are shown in Table 2.

[0139] (3) Friction and wear property test:

[0140] The Anton Paar multifunctional friction tester is used to analyze the tribological properties of the film, the atmospheric humidity is 50±5% RH, the test temperature is 25±3 ℃, the GCr15 steel ball is used as the friction pair, the reciprocating sliding mode is adopted, the frequency is 5 Hz, the sliding step is 5 mm, the running time is 1 h, and the normal load is 5 N. The contact type step meter is used to measure the wear volume, and the wear rate is obtained by dividing the wear volume by the load and the total sliding distance. The test results of the film friction coefficient and wear rate in the atmospheric room temperature environment are shown in Figure 6 .

[0141] Example 4

[0142] In this embodiment, the base material is 316 stainless steel and single crystal silicon wafer. Among them, the 316 stainless steel is used as the base material to deposit the molybdenum disulfide / tungsten diboride nano composite multilayer film, which can be used for service performance detection, including related mechanical properties, atmospheric room temperature friction performance test, etc. The single crystal silicon wafer is used as the base material to deposit the molybdenum disulfide / tungsten diboride nano composite multilayer film, which can be used for testing the thickness and structure of the film.

[0143] The non-equilibrium magnetron sputtering technology is used to prepare the molybdenum disulfide / tungsten diboride nano composite multilayer film on the surface of the substrate, which mainly includes the following steps:

[0144] The mechanically polished base material is placed in an acetone solution for ultrasonic cleaning for 15 minutes and dried with nitrogen. Then it is placed in an anhydrous ethanol solution for ultrasonic cleaning for 15 minutes and dried with nitrogen for standby.

[0145] The target position is arranged in a counterclockwise direction: two MoS2 targets (purity 99.9at.%), one Ti target (purity 99.99at.%), one MoS2 target (purity 99.9at.%), one WB2 target (purity 99.99at.%), and one MoS2 target (purity 99.99at.%).

[0146] The cleaned substrate is placed in a non-equilibrium magnetron sputtering chamber, and the vacuum degree is less than 3×10 -3 Pa, then high-purity argon gas is filled into the chamber, and then the target material is sputtered by argon plasma for 30 min with a substrate temperature of 100-120°C. The non-equilibrium magnetron sputtering technology is used to prepare the MoS2 / WB2 nano composite multilayer film with a sample holder rotation speed of 2 revolutions per minute. The specific steps are as follows:

[0147] (1) Substrate surface treatment: a bias voltage of -500V is applied to the substrate, and plasma etching is performed for 30 min with a substrate temperature of about 100°C to remove the surface oxide of the substrate.

[0148] (2) Ti transition layer deposition: Ti target current is 3.0A, substrate bias is -70V, working gas is argon, gas flow is 16sccm, substrate deposition temperature is 80°C, pressure is about 0.2Pa, deposition time is 1200s, Ti transition layer with a thickness of about 200nm is deposited on the substrate surface;

[0149] (3) Ti / MoS2 / WB2 gradient transition layer: the Ti target current is gradually reduced to 0 A, while the MoS2 target current is gradually increased to 1.6 A and the WB2 target current is gradually increased to 1.0 A, the working gas is Ar, the gas flow is 16 seem, the substrate bias is -50 V, the substrate deposition temperature is about 100 ℃, the pressure is about 0.2 Pa, the deposition time is 1800 s, and the Ti / MoS2 / WB2 gradient transition layer with a thickness of about 200 nm is deposited on the surface of the Ti transition layer;

[0150] (4) MoS2 / WB2 nanocomposite multilayer: the MoS2 target current is kept at 1.6 A and the WB2 target current is kept at 1.0 A, the remaining deposition parameters are kept unchanged, the deposition time is 7000 s, and the thickness modulation ratio of the MoS2 layer to the WB2 layer is controlled to be 3-4:1; wherein the thickness of the MoS2 single layer is about 6 nm, the thickness of the WB2 single layer is about 2 nm, the MoS2 / WB2 nanocomposite multilayer has a thickness of about 1.8 μm, and the total thickness of the MoS2 / WB2 nanocomposite multilayer is controlled to be about 2.7 μm.

[0151] The structure and mechanical properties of the MoS2 / WB2 nanocomposite multilayer film obtained by the above deposition are tested.

[0152] (1) Structure test results

[0153] Referring to Figure 1 The XRD test results of the MoS2 / WB2 nanocomposite multilayer film prepared in this embodiment show that the MoS2 / WB2 nanocomposite multilayer film grows in the MoS2(002) orientation with preferential growth.

[0154] Referring to 2b, the SEM image of the cross section of the film prepared in this embodiment shows that the Ti transition layer has a thickness of about 200 nm, the Ti / MoS2 / WB2 nanogradient transition layer has a thickness of about 200 nm, the MoS2 / WB2 nanocomposite multilayer has a thickness of about 2.5 μm, and the total thickness of the MoS2 / WB2 nanocomposite multilayer film is about 2.8 μm.

[0155] Referring to Figure 3b The cross-sectional TEM image of the MoS2 / WB2 nanocomposite multilayer film prepared in this embodiment shows that the interface between the layers in the image is almost invisible, indicating that mutual diffusion occurs between MoS2 and WB2, enhancing the interfacial bonding force and avoiding the occurrence of peeling under stress, thereby providing a structural basis for improving the tribological properties.

[0156] Referring to Figure 4bThe high-resolution TEM image of the MoS2 / WB2 nanocomposite multilayer film prepared in this embodiment shows that, in the MoS2 / WB2 nanocomposite multilayer film, the MoS2 layer has a thickness of about 6 nm; the WB2 layer has a thickness of about 2 nm; and the thickness modulation ratio of the MoS2 layer and the WB2 layer is controlled at 3:1.

[0157] (2) Mechanical property test:

[0158] The hardness and elastic modulus of the film were measured by using an MTS NanoIndenter G200 nanoindentation system, the indentation depth of the diamond indenter was 1 / 10 of the film thickness, six points were measured and averaged, and the test results are shown in Table 2.

[0159] (3) Friction and wear property test:

[0160] The tribological performance of the film was analyzed by using an Anton Paar multifunctional friction tester, the atmospheric humidity was 50±5% RH, and the test temperature was 25±3°C. A GCr15 steel ball was used as the friction pair, a reciprocating sliding mode was used, the frequency was 5 Hz, the sliding step was 5 mm, the running time was 1 h, and the normal load was 5 N. At the same time, the high-temperature tribological performance of the film was analyzed by using an Anton Paar multifunctional high-temperature friction tester, the test temperature was 100°C, 200°C, and 300°C, a GCr15 steel ball was used as the friction pair, a cyclic rotation mode was used, the linear speed was 12.56 cm / s, the rotation radius was 4 mm, the running time was 1 h, and the normal load was 5 N. The wear volume was measured by using a contact-type step meter, and the wear rate was obtained by dividing the wear volume by the load and the total sliding distance. The results of the test of the atmospheric room temperature environment friction coefficient and the wear rate of the film are shown in Table 3. Figure 6 The results of the test of the atmospheric high-temperature environment friction coefficient and the wear rate of the film are shown in Table 4. Figures 10-11

[0161] Example 5

[0162] In this embodiment, the substrate materials are 316 stainless steel and single crystal silicon wafer. The MoS2 / WB2 nanocomposite multilayer film deposited on the 316 stainless steel substrate material can be used for service performance detection, including related mechanical properties, atmospheric room temperature friction performance test, etc.; the MoS2 / WB2 nanocomposite multilayer film deposited on the single crystal silicon wafer substrate material can be used for the test of the thickness and structure of the film, etc.

[0163] The MoS2 / WB2 nanocomposite multilayer film was prepared on the substrate surface by using a non-equilibrium magnetron sputtering technique, mainly including the following steps:

[0164] ​The mechanically polished substrate material was placed in an acetone solution for ultrasonic cleaning for 15 minutes, and then dried with nitrogen. Subsequently, the substrate material was placed in an anhydrous ethanol solution for ultrasonic cleaning for 15 minutes, and then dried with nitrogen for standby use.

[0165] The target arrangement was set in a counterclockwise direction: two MoS2 targets (purity of 99.9 at.%), one Ti target (purity of 99.99 at.%), one MoS2 target (purity of 99.9 at.%), one WB2 target (purity of 99.99 at.%), and one MoS2 target (purity of 99.99 at.%).

[0166] The cleaned substrate was placed in a non-equilibrium magnetron sputtering chamber, and vacuumed to a vacuum degree of less than 3 x 10 -3 Pa, high-purity argon gas was filled into the chamber, and then the target material was cleaned by argon plasma sputtering for 30 minutes, with a substrate temperature of 100-120°C. The MoS2 / WB2 nanocomposite multilayer film was prepared by using a non-equilibrium magnetron sputtering technique, with a sample holder rotation speed of 2 revolutions per minute. The specific steps are as follows:

[0167] (1) Substrate surface treatment: a bias voltage of -500 V was applied to the substrate, and the substrate surface was etched by plasma for 30 minutes, with a substrate temperature of about 100°C, to remove the oxide on the substrate surface.

[0168] (2) Ti transition layer deposition: the Ti target current was 3.0 A, the substrate bias voltage was -70 V, the working gas was argon, the gas flow rate was 16 sccm, the substrate deposition temperature was 80°C, the pressure was about 0.2 Pa, and the deposition time was 1200 s, to deposit a Ti transition layer on the substrate surface, with a thickness of about 200 nm.

[0169] (3) Ti / MoS2 / WB2 gradient transition layer: the Ti target current was gradually reduced to 0 A, while the MoS2 target current was gradually increased to 1.6 A and the WB2 target current was gradually increased to 1.2 A, the working gas was Ar, the gas flow rate was 16 sccm, the substrate bias voltage was -50 V, the substrate deposition temperature was about 100°C, the pressure was about 0.2 Pa, and the deposition time was 1800 s, to deposit a Ti / MoS2 / WB2 gradient transition layer on the Ti transition layer surface, with a thickness of about 200 nm.

[0170] (4) MoS2 / WB2 nanocomposite multilayer: the MoS2 target current was maintained at 1.6 A, the WB2 target current was maintained at 1.2 A, and the remaining deposition parameters were maintained unchanged, the deposition time was 7000 s, the thickness modulation ratio of the MoS2 layer to the WB2 layer was controlled to be 3-4:1, the thickness of a single MoS2 layer was about 6 nm, the thickness of a single WB2 layer was about 2 nm, the thickness of the MoS2 / WB2 nanocomposite multilayer was about 1.8 μm, and the total thickness of the MoS2 / WB2 nanocomposite multilayer film was controlled to be about 2.9 μm.

[0171] The MoS2 / WB2 nanocomposite multilayer film obtained by the above deposition was tested as follows:

[0172] (1) Structure test:

[0173] Referring to Figure 1 The XRD test results of the MoS2 / WB2 nanocomposite multilayer film prepared in this embodiment show that the MoS2 / WB2 nanocomposite multilayer film grows preferentially in the MoS2(002) orientation.

[0174] (2) Mechanical property test results

[0175] The hardness and elastic modulus of the film were measured by MTS NanoIndenter G200 nanoindentation system, the indentation depth of the diamond indenter was 1 / 10 of the film thickness, six points were measured and averaged, and the test results are shown in Table 2.

[0176] (3) Friction and wear performance test:

[0177] The thin film was analyzed for tribological performance by an Anton Paar multifunctional friction tester, the atmospheric humidity was 50±5% RH, the test temperature was 25±3°C, a GCr15 steel ball was used as the friction pair, a reciprocating sliding mode was used, the frequency was 5 Hz, the sliding step was 5 mm, the running time was 1 h, and the normal load was 5 N. A contact-type step meter was used to measure the wear volume, and the wear rate was obtained by dividing the wear volume by the load and the total sliding distance. The test results of the atmospheric room temperature friction coefficient and the wear rate of the film are shown in Figure 6

[0178] Comparative Example 1

[0179] In this comparative example, the substrate materials are 316 stainless steel and single crystal silicon wafers. Among them, after the deposition of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film on the 316 stainless steel substrate material, the film can be used for service performance detection, including related mechanical properties, atmospheric room temperature friction performance test, etc.; after the deposition of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film on the single crystal silicon wafer substrate material, the film can be used for testing the thickness, structure, etc. of the film.

[0180] A pure molybdenum disulfide film was prepared on the surface of the substrate by using a non-equilibrium magnetron sputtering technique, mainly including the following steps:

[0181] The surface of the substrate was mechanically polished, the substrate material was placed in an acetone solution for ultrasonic cleaning for 15 minutes, and then dried with nitrogen; then placed in an anhydrous ethanol solution for ultrasonic cleaning for 15 minutes, and then dried with nitrogen.

[0182] ​The substrate after cleaning treatment was placed in a non-equilibrium magnetron sputtering chamber, vacuumed to a vacuum degree lower than 3x10 -3 Pa, high-purity argon gas was filled into the chamber, and the target material 30 was sputtered and cleaned by argon plasma for 30 min, and the substrate temperature was about 100-120°C. By using a non-equilibrium magnetron sputtering technology, a pure MoS2 film was prepared by controlling Ti target material (purity 99.99at.%) and MoS2 target material (purity 99.9at.%), and the sample holder rotation speed was set to 5 revolutions per minute. The specific steps are as follows:

[0183] (1) Substrate surface treatment: a bias voltage of -450V was applied to the substrate, and the substrate temperature was about 100°C. The substrate surface oxide was removed by plasma etching for 30 min.

[0184] (2) Ti transition layer deposition: Ti target current was 3.0A, substrate bias was -70V, working gas was argon, gas flow was 16sccm, substrate deposition temperature was 80°C, pressure was about 0.2Pa, and deposition time was 1200s. A Ti transition layer with a thickness of about 200nm was deposited on the substrate surface.

[0185] (3) Ti / MoS2 gradient transition layer: Ti target current was gradually reduced to 0A, while MoS2 target current was gradually increased to 1.6A, working gas was Ar, gas flow was 16sccm, substrate bias was -50V, substrate deposition temperature was about 100°C, pressure was about 0.2Pa, and deposition time was 1200s. A Ti / MoS2 transition layer with a thickness of about 200nm was deposited on the Ti transition layer surface.

[0186] (4) Pure MoS2 layer: MoS2 target current was kept at 1.6A, and the rest of the deposition parameters were unchanged. The thickness of the pure MoS2 film was controlled to be about 2.5μm by adjusting the deposition time.

[0187] The pure MoS2 film obtained by the above deposition was tested as follows:

[0188] (1) Structure test:

[0189] Referring to Figure 1 The XRD test results of the pure MoS2 film prepared in this comparative example showed that the MoS2(002) orientation of the pure MoS2 film did not grow obviously.

[0190] (2) Mechanical property test:

[0191] The hardness and elastic modulus of the film were measured by MTS NanoIndenter G200 nanoindentation system. The indentation depth of the diamond indenter was 1 / 10 of the film thickness, and the average value of six points was measured. The test results are shown in Table 2.

[0192] (3) Friction and wear performance test:

[0193] The thin films were analyzed for tribological properties using an Anton Paar multi-functional friction tester, with atmospheric humidity of 50±5% RH and a test temperature of 25±3°C. A GCr15 steel ball was used as the friction pair, with a reciprocating sliding mode, a frequency of 5 Hz, a sliding step of 5 mm, a running time of 1 h, and a normal load of 5 N. Meanwhile, the thin films were analyzed for high-temperature tribological properties using an Anton Paar multi-functional high-temperature friction tester, with a test temperature of 100°C, 200°C, or 300°C, a GCr15 steel ball used as the friction pair, a cyclic rotation mode, a linear velocity of 12.56 cm / s, a rotation radius of 4 mm, a running time of 1 h, and a normal load of 5 N. A contact-type step meter was used to measure the wear volume, and the wear volume was divided by the load and the total sliding distance to obtain the wear rate. The results of the test of the friction coefficient and the wear rate of the thin films in an atmospheric room-temperature environment are shown in Figure 6 The results of the test of the friction coefficient and the wear rate of the thin films in an atmospheric high-temperature environment are shown in Figure 10 and Figure 11

[0194] As can be seen from Table 1, the deposited thin films are mainly MoS2, meeting the functional requirements of lubricating thin films; the WB2 interlayer as a bearing layer can improve the hardness and the hardness / elasticity ratio of the thin films, which is conducive to obtaining excellent tribological properties.

[0195] The hardness and the elastic modulus of the six thin film samples in Examples 1-5 and Comparative Example 1 were measured by using the MTS NanoIndenter G200 nanoindentation instrument system to press six points on the surface of each sample to a depth of 200 nm. The results are shown in Table 1. As can be seen from Table 1, the hardness of the molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films is greater than that of the pure molybdenum disulfide thin film.

[0196] Table 1 Hardness, elastic modulus, and hardness / elasticity ratio of Examples 1-5 and Comparative Example 1

[0197]

[0198] As shown in Table 2, the average friction coefficient of the six thin films of Examples 1-5 (MoS2 / WB2) and Comparative Example 1 (MoS2) in an atmospheric environment at room temperature.

[0199] As shown in Table 3, the average wear rate of the thin films obtained in Examples 1-5 (MoS2 / WB2) and Comparative Example 1 (MoS2) in an atmospheric environment at room temperature. Referring to Figure 5 is a friction curve diagram of the MoS2 / WB2 nanocomposite multilayer thin films prepared in Examples 1-5 and the pure MoS2 thin film prepared in Comparative Example 1 in an atmospheric room-temperature environment.

[0200] Referring to​Figure 6 is the average friction coefficient column chart and the corresponding wear rate column chart of the MoS2 / WB2 nanocomposite multilayer film prepared by the embodiments 1-5 of the present application and the pure MoS2 film prepared by the comparative example 1 under the atmospheric room temperature environment.

[0201] From the results of the above chart, the average wear rate of the embodiments 1-5 (MoS2 / WB2) under the atmospheric room temperature environment is lower than that of the comparative example 1 (MoS2); wherein the embodiment 4 has the best friction performance under the atmospheric room temperature environment, and the wear rate is stably at 1.88x10 -7 mm 3 / N·m.

[0202] Referring to Figures 7-9 is the friction coefficient curve chart of the MoS2 / WB2 nanocomposite multilayer film prepared by the embodiment 4 of the present application and the pure MoS2 film prepared by the comparative example 1 under the atmospheric high temperature environment (100℃, 200℃, 300℃ respectively). The MoS2 / WB2 nanocomposite multilayer film with the WB2 target current of 1.0A in the embodiment 4 has relatively stable friction performance at 100℃, 200℃ and 300℃.

[0203] Referring to Figure 10 is the average friction coefficient column chart of the MoS2 / WB2 nanocomposite multilayer film prepared by the embodiment 4 of the present application and the pure MoS2 film prepared by the comparative example 1 under the atmospheric high temperature environment (100-300℃). The MoS2 / WB2 nanocomposite multilayer film with the WB2 target current of 1.0A in the embodiment 4 has the best friction coefficient at 100℃, 200℃ and 300℃.

[0204] Referring to Figure 11 is the wear rate column chart of the MoS2 / WB2 nanocomposite multilayer film prepared by the embodiment 4 of the present application and the pure MoS2 film prepared by the comparative example 1 under the atmospheric high temperature environment (100-300℃). The MoS2 / WB2 nanocomposite multilayer film with the WB2 target current of 1.0A in the embodiment 4 has the lowest wear rate at 100℃, 200℃ and 300℃.

[0205] From the above results, the MoS2 / WB2 nanocomposite multilayer film with the WB2 target current of 1.0A in the embodiment 4 has the lowest wear rate at 100℃, 200℃ and 300℃.

[0206] Table 2 The friction coefficient of the embodiments 1-5 of the present application and the comparative example 1 under the atmospheric room temperature

[0207]

[0208] Table 3 Wear rate (x 10 -7 mm 3 / N·m)

[0209]

[0210] Aspects, embodiments, features, and examples of the present application should be considered in all respects as illustrative only and not restrictive, the scope of the application being indicated by the appended claims. Other embodiments, modifications, and uses thereof will be apparent to those skilled in the art, without departing from the spirit and scope of the application as defined in the following claims.

[0211] The use of headings and sections in the present application is not meant to limit the application; each section can apply to any aspect, embodiment, or feature of the present application.

[0212] Throughout this application, where compositions are described as having, containing, or including certain components, it is contemplated that the application teachings also consist essentially of, and can consist of, those components unless otherwise specified. Where processes are described, similar principles apply and the process as described can be essentially consists of, or consist of, the

[0213] The use of the terms "include," "includes," "including," "have," "has," "having," or "comprises," "comprising," "comprise" or "comprising" is generally understood as meaning "including." Unless otherwise specified, the use of the singular includes the plural.

[0214] It should be understood that the order of steps or order for performing certain actions is immaterial so long as the application teachings remains operable. Moreover, two or more steps or actions can be conducted simultaneously.

[0215] In addition, the present inventors have tested the aforementioned examples with other raw materials, process operations, process conditions described in the specification, and all have obtained relatively ideal results.

[0216] While the application has been described with reference to the illustrative embodiments, those skilled in the art will understand that various other changes, omissions, and / or additions can be made without departing from the spirit and scope of the application. Further, many modifications can be made to adapt a particular situation or material to the teachings of the application without departing from its scope. Therefore, it is intended that the application not be limited to the disclosed embodiments, but will include all embodiments falling within the scope of the appended claims. Moreover, unless specifically stated otherwise, any use of the terms first, second, etc., does not denote any ordinal, or importance, but merely distinguishes one element from another.

Claims

1. A molybdenum disulfide / tungsten diboride nanocomposite multilayer film, using unbalanced magnetron sputtering technology, comprising sequentially depositing a titanium transition layer, a titanium / molybdenum disulfide / tungsten diboride gradient transition layer, and a molybdenum disulfide / tungsten diboride nanocomposite multilayer film in its thickness direction; The target current applied to the titanium target gradually decreased from the working current of 3.0~5.0 A to 0, the target current applied to the molybdenum disulfide target gradually increased from 0 to the working current of 1.6 A, and the target current applied to the tungsten diboride target gradually increased from 0 to the working current of 0.4 A~1.2 A. The substrate bias voltage was -50~-70 V, the working gas flow rate was 12~16 sccm, the chamber temperature was 80~120 ℃, the reaction chamber pressure was 0.1~0.4 Pa, and the deposition time was 1200~1800 s. The target current applied to the molybdenum disulfide target is 1.6 A; the target current applied to the tungsten diboride target is 0.4 A, 0.6 A, 0.8 A, 1.0 A, or 1.2 A; the substrate bias voltage is -50 to -70 V; the rotation speed of the rotating frame is 2 revolutions; the working gas flow rate is 12 to 16 sccm; the substrate temperature is 80 to 120 ℃; the reaction chamber pressure is 0.1 to 0.4 Pa; and the deposition time is 6000 to 8000 s. The total thickness of molybdenum disulfide / tungsten diboride within one modulation cycle is less than 10 nm. The unbalanced magnetron sputtering technique used enables the mutual diffusion between molybdenum disulfide and tungsten diboride, which have nanoscale effects, promoting the fusion of the interface between the molybdenum disulfide layer and the tungsten diboride layer, resulting in a thin film with good interfacial bonding.

2. The molybdenum disulfide / tungsten diboride nanocomposite multilayer thin film according to claim 1, characterized in that, The molybdenum disulfide / tungsten diboride nanocomposite multilayer film has a boron atom content of 16.7% and a W content of 10.7%.

3. The molybdenum disulfide / tungsten diboride nanocomposite multilayer thin film according to claim 1, characterized in that, The thickness of the titanium transition layer is 100~300 nm.

4. The molybdenum disulfide / tungsten diboride nanocomposite multilayer thin film according to claim 1, characterized in that, The thickness of the titanium / molybdenum disulfide / tungsten diboride gradient transition layer is 200~300 nm.

5. The molybdenum disulfide / tungsten diboride nanocomposite multilayer thin film according to claim 1, characterized in that, The thickness of the molybdenum disulfide / tungsten diboride nanocomposite multilayer is 2.1 μm to 2.8 μm.

6. The molybdenum disulfide / tungsten diboride nanocomposite multilayer thin film according to claim 1, characterized in that, The surface roughness of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film is less than 8 nm.

7. The molybdenum disulfide / tungsten diboride nanocomposite multilayer thin film according to claim 1, characterized in that, The molybdenum disulfide / tungsten diboride nanocomposite multilayer film has a friction coefficient of 0.06~0.12 and a wear rate of 1.88×10⁻⁶ at room temperature. -7 ~1.58×10 -6 mm 3 / N·m.

8. The molybdenum disulfide / tungsten diboride nanocomposite multilayer thin film according to claim 1, characterized in that, The molybdenum disulfide / tungsten diboride nanocomposite multilayer film exhibits a friction coefficient of 0.02~0.16 and a wear rate of 3.62×10⁻⁶ under atmospheric conditions of 100 °C. -7 ~1.09×10 -6 mm 3 / N·m; the coefficient of friction is 0.04~0.20 at 200 ℃, and the wear rate is 3.96×10 -7 ~1.70×10 -6 mm 3 / N·m; the coefficient of friction is 0.07~0.50 at 300 ℃, and the wear rate is 9.30×10 -7 ~1.27×10 -5 mm 3 / N·m.

9. A method for preparing a molybdenum disulfide / tungsten diboride nanocomposite multilayer thin film as described in any one of claims 1-8, characterized in that, The preparation method includes using unbalanced magnetron sputtering technology to sequentially deposit a titanium transition layer, a titanium / molybdenum disulfide / tungsten diboride gradient transition layer, and a molybdenum disulfide / tungsten diboride nanocomposite multilayer on the surface of a substrate to obtain the molybdenum disulfide / tungsten diboride nanocomposite multilayer film. The host phase, molybdenum disulfide, preferentially grows along the (002) crystal plane parallel to the matrix.

10. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films according to claim 9, characterized in that, The unbalanced magnetron sputtering technology is based on a six-target technique for deposition, which includes two molybdenum disulfide targets, one titanium metal target, two molybdenum disulfide targets, and one tungsten diboride target arranged in a counterclockwise direction.

11. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films according to claim 9, characterized in that, Unbalanced magnetron sputtering technology is used, with a titanium metal target as the cathode target and argon gas as the working gas. A target current is applied to the titanium metal target, and a negative bias voltage is applied to the substrate, thereby depositing the titanium transition layer on the substrate surface. The target current is 3.0~5.0 A, the substrate bias voltage is -70~-90 V, the working gas flow rate is 12~16 sccm, the deposition chamber pressure is 0.1~0.4 Pa, and the deposition time is 1200~1800 s.

12. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films according to claim 9, characterized in that, The thickness of the titanium transition layer is 100~300 nm.

13. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films according to claim 9, characterized in that, Unbalanced magnetron sputtering technology is used, with titanium, molybdenum disulfide, and tungsten diboride targets as cathode targets and argon as the working gas. Target current is applied to the titanium, molybdenum disulfide, and tungsten diboride targets, and a negative bias voltage is applied to the substrate, thereby depositing a titanium / molybdenum disulfide / tungsten diboride gradient transition layer on the surface of the titanium transition layer.

14. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films according to claim 9, characterized in that, The thickness of the titanium / molybdenum disulfide / tungsten diboride gradient transition layer is 100~300 nm.

15. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayers according to claim 9, characterized in that, Unbalanced magnetron sputtering technology was employed with molybdenum disulfide (MoDS) and tungsten diboride (TBD) targets as cathode materials and argon as the working gas. Target currents were applied to the MoDS and TBD targets respectively, and a negative bias voltage was applied to the substrate. The rotation speed of the rotating frame was controlled to achieve uniform growth and interdiffusion between the MoDS and TBD layers. A MoDS / TBD nanocomposite multilayer film was deposited on the surface of the titanium / MoDS / TBD gradient transition layer.

16. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films according to claim 9, characterized in that, The operating current of the target current applied to tungsten diboride is 0.6A~1.2A.

17. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films according to claim 15, characterized in that, The target current applied to tungsten diboride is 1.0 A or 1.2 A.

18. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films according to claim 9, characterized in that, The thickness of the molybdenum disulfide / tungsten diboride nanocomposite multilayer film is 2.6~2.8 μm.

19. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films according to claim 9, characterized in that, In the molybdenum disulfide / tungsten diboride nanocomposite multilayer film, the thickness of the molybdenum disulfide layer is greater than the thickness of the tungsten diboride layer.

20. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films according to claim 9, characterized in that, The thickness modulation ratio of the molybdenum disulfide layer and the tungsten diboride layer is controlled at 3~4:

1.

21. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films according to claim 9, characterized in that, Also includes: The deposition chamber was evacuated to a vacuum level of 3 × 10⁻⁶. -3 Below Pa, the treated substrate is first subjected to argon plasma etching.

22. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films according to claim 21, characterized in that, The argon plasma etching process includes: applying a substrate bias voltage of -400 to -500 V for an etching time of 1800 s.

23. The method for preparing molybdenum disulfide / tungsten diboride nanocomposite multilayer thin films according to claim 9, characterized in that, The substrate is made of at least one of the following materials: 9Cr18, T6Al4V, 316 stainless steel, and monocrystalline silicon wafer.

24. Use of a molybdenum disulfide / tungsten diboride nanocomposite multilayer film according to any one of claims 1-8 in the field of surface protection of aerospace components; said use includes application to the surface of critical moving parts of aerospace machinery.

25. The use of a molybdenum disulfide / tungsten diboride nanocomposite multilayer film according to any one of claims 1-8 in the field of substrate surface protection for nuclear power bearings; wherein the substrate material is selected from any one of single-crystal silicon wafers, T6Al4V, 316 stainless steel, and 9Cr18.

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