A low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film, its preparation method and application

Abstract

This invention provides a low-friction, wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film, its preparation method, and its applications, relating to the field of protective coating materials technology. The low-friction, wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film provided by this invention comprises alternating layers of TiNbMoTaCr nanolayers and MoS2 nanolubricating layers; the TiNbMoTaCr nanolayers have a hybrid structure of amorphous and nanocrystalline materials; the MoS2 nanolubricating layer comprises bent MoS2 nanosheets. Using the low-friction, wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film provided by this invention as a protective coating for metals can significantly reduce the coefficient of friction of the material and improve the frictional stability and durability of the metal material.

Description

Technical Field

[0001] This invention relates to the field of protective coating materials technology, specifically to a low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film, its preparation method, and its application. Background Technology

[0002] With the rapid development of aerospace technology and industrial equipment, moving parts made of titanium alloys are subjected to more severe friction and wear. Due to their susceptibility to adhesive wear, they exhibit high coefficients of friction and severe wear problems, seriously affecting the service safety and durability of related components. Therefore, introducing low-friction and wear-resistant protective coatings onto the surface of titanium alloys is of great significance for significantly improving working efficiency and service life.

[0003] High-entropy alloys typically contain four or more metallic elements in equiatomic or near-equiatomic ratios. This abundance of elements contributes to the system's high mixing entropy and stable Gibbs free energy. Extensive research has shown that refractory high-entropy alloys exhibit many superior properties, including high strength, high hardness, excellent corrosion resistance, and thermal stability. Furthermore, refractory high-entropy alloys possess good interfacial adhesion and mechanical compatibility with the metal matrix. These excellent combined properties make refractory high-entropy alloys a promising candidate for protective coatings against inevitable friction and harsh environmental corrosion. However, existing high-entropy alloy protective layers exhibit high and unstable coefficients of friction. Summary of the Invention

[0004] The purpose of this invention is to provide a low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film, its preparation method, and its application. Using the low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film provided by this invention as a protective coating for metals can significantly reduce the coefficient of friction of the material and improve the frictional stability and durability of the metal material.

[0005] To achieve the above-mentioned objectives, the present invention provides the following technical solution:

[0006] This invention provides a low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film, comprising alternating layers of TiNbMoTaCr nanolayers and MoS2 nano-lubricating layers; the TiNbMoTaCr nanolayers have a hybrid structure of amorphous and nanocrystalline materials; the MoS2 nano-lubricating layer comprises bent MoS2 nanosheets.

[0007] Preferably, a modulation unit is formed by stacking a TiNbMoTaCr nanolayer and a MoS2 nano-lubricating layer in sequence, and the number of modulation units of the low-friction and wear-resistant TiNbMoTaCr / MoS2 nano-multilayer film is 40 to 80; the thickness ratio of the TiNbMoTaCr nanolayer and the MoS2 nano-lubricating layer in each modulation unit is independently 10:5 to 10.

[0008] Preferably, the thickness of each TiNbMoTaCr nanolayer is 5–20 nm; the thickness of each MoS2 nanolubricating layer is 5–10 nm.

[0009] This invention provides a method for preparing the low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayered film described above, comprising the following steps:

[0010] Using magnetron sputtering technology, TiNbMoTaCr composite target and MoS2 target were used as sputtering targets to alternately sputter the substrate to obtain a low-friction and wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film.

[0011] Preferably, the TiNbMoTaCr composite target is composed of Ti target, Nb target, Mo target, Ta target and Cr target spliced ​​together.

[0012] Preferably, the TiNbMoTaCr composite target uses a DC power supply; the sputtering current of the TiNbMoTaCr composite target is 0.2 to 0.4 A; and the distance between the TiNbMoTaCr composite target and the substrate is 60 to 80 mm.

[0013] Preferably, the MoS2 target uses a DC power supply or a radio frequency power supply.

[0014] Preferably, when the MoS2 target uses a DC power supply, the DC sputtering current of the MoS2 target is 0.2 to 0.3 A; when the MoS2 target uses an RF power supply, the RF sputtering power of the MoS2 target is 30 to 100 W.

[0015] The distance between the MoS2 target and the substrate is 60–80 mm.

[0016] Preferably, before the alternating sputtering, the substrate temperature is set to 200–400°C.

[0017] This invention provides the application of the low-friction and wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film described in the above technical solution or the low-friction and wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film prepared by the preparation method described in the above technical solution as a protective coating.

[0018] This invention provides a low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film, comprising alternating layers of TiNbMoTaCr nanolayers and MoS2 nano-lubricating layers. The TiNbMoTaCr nanolayers have a hybrid structure of amorphous and nanocrystalline materials. The MoS2 nano-lubricating layer comprises bent MoS2 nanosheets. In this invention, the TiNbMoTaCr nanolayers possess high hardness, providing mechanical support; the unique low-shear structure of MoS2 exhibits excellent lubricity. The TiNbMoTaCr / MoS2 nanolayer film constructed in this invention combines the advantages of each nanolayer and, through the synergistic effect of the nanolayers, integrates high hardness and excellent tribological properties to obtain a low-friction, wear-resistant integrated film. Simultaneously, the self-assembled MoS2@metal oxide nanoroll structure formed at the friction interface constitutes a stable multi-point contact configuration, altering the contact mode of the sliding interface and effectively reducing frictional resistance and sliding contact area. The low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film provided by this invention combines high hardness with excellent tribological properties, serving as a low-friction, wear-resistant protective coating and solving the problem of adhesive wear on metal surfaces. Using the low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film provided by this invention as a protective coating for metals can significantly reduce the coefficient of friction and improve the frictional stability and durability of metal materials.

[0019] The low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film provided by this invention has the following beneficial effects:

[0020] (1) The high entropy effect and lattice distortion of the TiNbMoTaCr nanolayer in the low friction and wear-resistant TiNbMoTaCr / MoS2 nanolayer film provided by the present invention endow it with high hardness. The large number of layer interfaces and the amorphous / nanocrystalline mixed structure are beneficial to hinder the movement of dislocations, thereby making the TiNbMoTaCr nanolayer exhibit a supporting role.

[0021] (2) The low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film provided by this invention contains a large number of low-shear surfaces in the MoS2 nano-lubricating layer composed of bent MoS2 nanosheets, which can alleviate the high shear effect at the friction interface through intragranular sliding between the low-shear surfaces of MoS2. Furthermore, the bent structure extends the two-dimensional nanosheets to three dimensions, which is beneficial to improving the hardness and oxidation resistance of MoS2.

[0022] (3) In the low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film provided by this invention, during the friction process, the oxide generated by the oxidation of the metal and the bent layer of MoS2 are interlocked. Under the induction of external force, the atomic planes of the two in contact move at a speed lower than the sliding speed between the intramolecular layers of MoS2, gradually forming a nano-scroll structure. This leads to the formation of a self-assembled MoS2@metal oxide nano-scroll structure on the sliding contact surface, creating a stable multi-point contact configuration. This changes the contact mode of the sliding interface, effectively reducing frictional resistance and sliding contact area, resulting in a low coefficient of friction and wear rate for the TiNbMoTaCr / MoS2 nanolayer film. The results of the examples show that the coefficient of friction of the low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film provided by this invention is 0.08–0.48, and the wear rate is 9.561 × 10⁻⁶. -8 mm 3 / Nm~1.414×10 -6 mm 3 / Nm; Using the nano-multilayer film provided by this invention as a protective coating for metals can significantly reduce the coefficient of friction of materials and improve the frictional stability and durability of metal materials.

[0023] This invention provides a method for preparing the low-friction and wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film described in the above technical solution. This invention employs a multi-target magnetron sputtering layered deposition technique, which alternately introduces multiple nanomultilayer film deposition units with different thickness modulation ratios (the thickness ratio of the two nanolayers within a modulation unit) during deposition. This achieves control over the friction coefficient and wear rate, not only solving the problem of easy adhesive wear caused by the high shear force at the metal friction interface and improving macroscopic lubricity, but also utilizing the self-assembled MoS2@metal oxide nanorolls to achieve a stable multi-point contact configuration, changing the contact mode of the sliding interface, effectively reducing frictional resistance and sliding contact area, and reducing the wear rate of the TiNbMoTaCr / MoS2 nanomultilayer film. Attached Figure Description

[0024] Figure 1 This is a schematic diagram illustrating the preparation of a low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film according to the present invention.

[0025] Figure 2 (a) Friction coefficient curve and (b) Wear rate bar chart of the samples prepared in the embodiments and comparative examples of the present invention;

[0026] Figure 3 A cross-sectional TEM image of the sample prepared in Example 1 of this invention;

[0027] Figure 4 The image shows the HRTEM image of the wear debris from the sample prepared in Example 1 of this invention. Detailed Implementation

[0028] This invention provides a low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film, comprising alternating layers of TiNbMoTaCr nanolayers and MoS2 nano-lubricating layers; the TiNbMoTaCr nanolayers have a hybrid structure of amorphous and nanocrystalline materials; the MoS2 nano-lubricating layer comprises bent MoS2 nanosheets.

[0029] In this invention, a modulation unit is defined by a TiNbMoTaCr nanolayer and a MoS2 nano-lubricating layer stacked sequentially. The number of modulation units in the low-friction and wear-resistant TiNbMoTaCr / MoS2 nano-multilayer film is preferably 40 to 80, and more preferably 50 or 66. The thickness ratio of the TiNbMoTaCr nanolayer and the MoS2 nano-lubricating layer in each modulation unit is preferably 10:5 to 10, and more preferably 10:5 or 10:10.

[0030] In this invention, the elements in the TiNbMoTaCr nanolayer are in a near equimolar ratio.

[0031] In this invention, the thickness of each TiNbMoTaCr nanolayer is preferably 5–20 nm, more preferably 10–15 nm; the thickness of each MoS2 nanolubricating layer is preferably 5–10 nm, more preferably 6–8 nm. This invention limits the thickness of the TiNbMoTaCr nanolayer and the MoS2 nanolubricating layer to the above ranges to confine the excessive growth of TiNbMoTaCr and MoS2 at an appropriate nanoscale, inducing the preferential growth of low-shear surfaces of MoS2 through numerous multilayer interfaces and forming sufficiently curved sheet-like structures of MoS2, thus providing a basis for the formation of self-assembled MoS2@metal oxide nanoscroll structures.

[0032] In this invention, the TiNbMoTaCr nanolayer in the first modulation unit of the low-friction and wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film is preferably in contact with the substrate; the outermost layer of the low-friction and wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film is preferably a MoS2 nanolubricating layer.

[0033] This invention provides a method for preparing the low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayered film described above, comprising the following steps:

[0034] Using magnetron sputtering technology, TiNbMoTaCr composite target and MoS2 target were used as sputtering targets to alternately sputter the substrate to obtain a low-friction and wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film.

[0035] In this invention, the substrate is preferably a titanium sheet. In this invention, the substrate is preferably pretreated before use. In this invention, the pretreatment preferably includes sequential cleaning and drying. In this invention, the cleaning preferably includes ultrasonic cleaning for 20 minutes each using acetone and anhydrous ethanol in an ultrasonic cleaner. In this invention, the drying preferably includes drying the substrate with dry nitrogen gas.

[0036] In this invention, the sputtering gas used in the magnetron sputtering is preferably argon. The purity of the argon is preferably 99.995–99.999%, and the flow rate is preferably 50–80 sccm, more preferably 60–70 sccm.

[0037] In this invention, before performing the alternating sputtering, the vacuum level inside the magnetron sputtering system's coating chamber is preferably better than 8 × 10⁻⁶. -4 Pa. This invention maintains the vacuum level in the coating chamber of the magnetron sputtering system within the above-mentioned range, thereby maximizing the removal of gaseous impurities from the coating chamber and preventing sample contamination during the coating process.

[0038] In this invention, before the alternating sputtering, the substrate temperature is preferably set to 200–400°C, more preferably 300–350°C. By limiting the substrate temperature to this range, this invention promotes the formation of higher-quality thin films by sputtered particles on the substrate surface.

[0039] In this invention, during the alternating sputtering process, it is preferable to maintain substrate rotation. In this invention, the substrate rotation speed is 3–10 r / min, more preferably 5–8 r / min. Maintaining substrate rotation within this range enables the formation of a uniform thin film.

[0040] In this invention, the working pressure of the alternating sputtering process is preferably 0.6–1.5 Pa, more preferably 0.8–1.0 Pa. Using the above-mentioned working pressure ensures that the deposition rate reaches its optimal level.

[0041] In this invention, the diameter of the TiNbMoTaCr composite target is preferably 60 mm, and the purity is preferably 99.999%. In this invention, the TiNbMoTaCr composite target is preferably composed of Ti, Nb, Mo, Ta, and Cr targets joined together. In this invention, the TiNbMoTaCr composite target is preferably composed of five fan-shaped Ti, Nb, Mo, Ta, and Cr targets of the same size joined together.

[0042] In this invention, the TiNbMoTaCr composite target preferably uses a DC power supply; the sputtering current of the TiNbMoTaCr composite target is preferably 0.2 to 0.4 A, more preferably 0.3 A; and the sputtering voltage of the TiNbMoTaCr composite target is preferably 200 to 400 V, more preferably 304 V.

[0043] In this invention, the distance between the TiNbMoTaCr composite target and the substrate is preferably 60-80 mm, more preferably 70-75 mm.

[0044] In this invention, the single sputtering time of the TiNbMoTaCr composite target is preferably 5 to 15 s, more preferably 10 s.

[0045] In this invention, the diameter of the MoS2 target is preferably 60 mm, and the purity is preferably 99.999%.

[0046] In this invention, the MoS2 target preferably uses a DC power supply or an RF power supply. When the MoS2 target uses a DC power supply, the DC sputtering current of the MoS2 target is preferably 0.2–0.3 A; the DC sputtering voltage of the MoS2 target is preferably 300–600 V, more preferably 533 V. In this invention, when the MoS2 target uses an RF power supply, the RF sputtering power of the MoS2 target is preferably 30–100 W. By controlling the current maintained during sputtering within the above range, this invention enables precise control of the layer thickness.

[0047] In this invention, the distance between the MoS2 target and the substrate is preferably 60-80 mm, more preferably 70-75 mm.

[0048] In this invention, the single sputtering time of the MoS2 target is preferably 10-30 s, more preferably 13-26 s.

[0049] In a specific embodiment of the present invention, sputtering gas is introduced during the deposition of a low-friction, wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film, the working pressure in the deposition chamber is adjusted, the current of the sputtering power supply is set, and the target baffle is controlled to alternately face the TiNbMoTaCr composite target and the MoS2 target, thereby obtaining a modulation unit on the substrate surface in which TiNbMoTaCr nanolayers and MoS2 nanolubricating layers are deposited sequentially. Then, a continuous nanomultilayer film structure is formed by the accumulation of the modulation unit.

[0050] Preferably, after the sputtering is completed, the resulting film is cooled to room temperature under vacuum conditions to obtain a low-friction and wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film.

[0051] In a specific embodiment of the present invention, the preparation method of the low-friction, wear-resistant TiNbMoTaCr / MoS2 nanolayer film is as follows: Figure 1 As shown, this invention utilizes magnetron sputtering technology to first obtain a TiNbMoTaCr nanolayer with an amorphous / nanocrystalline hybrid structure on a substrate. Then, a MoS2 nano-lubricating layer composed of bent MoS2 nanosheets is deposited on the TiNbMoTaCr nanolayer. A modulation unit is formed by sequentially depositing one TiNbMoTaCr nanolayer and one MoS2 nano-lubricating layer, and the modulation units are repeatedly accumulated by alternately depositing TiNbMoTaCr nanolayers and MoS2 nano-lubricating layers to obtain the low-friction, wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film. This invention enables the control of the film's friction coefficient and wear rate, providing a fundamental support for integrating the frictional stability, macroscopic lubricity, and durability of multilayer films. The preparation method provided by this invention not only solves the problem of easy adhesive wear caused by the high shear force at the metal friction interface, improving macroscopic lubricity, but also achieves a stable multi-point contact configuration by utilizing self-assembled MoS2@metal oxide nanorolls, changing the contact mode of the sliding interface, effectively reducing frictional resistance and sliding contact area, and reducing the wear rate of the TiNbMoTaCr / MoS2 nanomultilayer film.

[0052] The present invention provides the application of the low-friction and wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film described in the above technical solution or the low-friction and wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film prepared by the preparation method described in the above technical solution as a protective coating, preferably as a metal protective coating.

[0053] The technical solutions of this invention will be clearly and completely described below with reference to the embodiments thereof. Obviously, the described embodiments are only a part of the embodiments of this invention, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0054] Example 1

[0055] The titanium sheet was ultrasonically cleaned for 20 minutes in an ultrasonic cleaner with acetone and anhydrous ethanol respectively. The titanium sheet was then dried with dry nitrogen to obtain a clean substrate, which was then mounted on the substrate holder. The TiNbMoTaCr composite target was mounted on target position 1 and the MoS2 target was mounted on target position 2. The substrate holder was placed on the sample holder and the target-substrate distance was adjusted to 70 mm.

[0056] After preparation is complete, close the vacuum chamber and evacuate to a vacuum level better than 8×10⁻⁶. -4 Pa;

[0057] Once the required vacuum level is reached, start the sample holder rotation, set the rotation speed of the sample holder to 5 r / min, and set the substrate temperature to 300℃.

[0058] After the substrate temperature reaches the set value, the argon gas flow rate is set to 70 sccm. The gas path valve is opened, and the regulating valve is used to adjust the working gas pressure in the vacuum coating chamber to 0.8 Pa. The DC power switch is turned on, and the current value of the TiNbMoTaCr composite target at target position 1 is adjusted to 0.3 A and the voltage value to 304 V; the current value of the MoS2 target at target position 2 is adjusted to 0.3 A and the voltage value to 533 V. After the glow discharge stabilizes, the target baffle control program is set. Target baffle 1 is opened so that target position 1 faces the substrate for 10 seconds, during which time target baffle 2 blocks target position 2. Then, target baffle 2 is opened so that target position 2 faces the substrate for 26 seconds, during which time target baffle 1 blocks target position 1. This cycle is repeated 50 times. After the cycle ends, the sample baffle is closed.

[0059] After deposition is complete, turn off the current to the TiNbMoTaCr composite target at target site 1 and the MoS2 target at target site 2, stop the argon gas supply, shut off the sample heating system, turn the modulation gate valve to its maximum, and wait for the sample heating temperature controller to display a temperature drop to room temperature before removing the sample. Then, alternately deposit the sample onto a titanium sheet to obtain l TiNbMoTaCr =10nm, l MoS2 =10 nm TiNbMoTaCr / MoS2 nanolayer film; where l TiNbMoTaCr Represents the thickness of each TiNbMoTaCr nanolayer, l MoS2 This represents the thickness of each MoS2 nano-lubricant layer.

[0060] The l obtained in this embodiment MoS2 Friction experiments were conducted on a 10 nm TiNbMoTaCr / MoS2 nanolayer film. The friction coefficient curve and wear rate are shown below. Figure 2 As shown, its coefficient of friction is 0.08, and its wear rate is 9.561 × 10⁻⁶. -8 mm 3 / Nm. l MoS2 The friction coefficient curve of the 10 nm TiNbMoTaCr / MoS2 nanomultilayer film remained low and stable, indicating that the prepared multilayer film has excellent tribological properties of low friction and wear resistance.

[0061] l MoS2 Cross-sectional TEM image of a 10 nm TiNbMoTaCr / MoS2 nanomultilayer film. Figure 3 As shown, the image contains a clear texture with alternating light and dark areas, confirming that l MoS2A 10 nm multilayer film was grown with a clearly defined layered structure, where the dark layer is a TiNbMoTaCr nanolayer and the bright layer is a MoS2 nano-lubricating layer. Figure 3 The magnified view on the right reveals that the brighter MoS2 nano-lubricating layer is not composed of a complete two-dimensional nanosheet structure, but rather of a large number of fragmented, short, and curved MoS2 sheet-like nanostructures (marked in red); while the darker TiNbMoTaCr nanolayer is composed of an amorphous / nanocrystalline blend structure.

[0062] After the friction experiment, l MoS2 HRTEM (High Resolution Transmission Electron Microscopy) image of wear debris at the sliding interface of a 10 nm TiNbMoTaCr / MoS2 nanolayer film. Figure 4 As shown, the wear debris in the sliding contact area forms a self-assembled MoS2 nanoroll structure encapsulating metal oxides, creating a stable multi-point contact configuration. This alters the contact mode of the sliding interface, effectively reducing frictional resistance and sliding contact area, and thus lowering the wear rate of the TiNbMoTaCr / MoS2 nanolayer film.

[0063] Example 2

[0064] The titanium sheet was ultrasonically cleaned for 20 minutes in an ultrasonic cleaner with acetone and anhydrous ethanol respectively. The titanium sheet was then dried with dry nitrogen to obtain a clean substrate, which was then mounted on the substrate holder. The TiNbMoTaCr composite target was mounted on target position 1 and the MoS2 target was mounted on target position 2. The substrate holder was placed on the sample holder and the target-substrate distance was adjusted to 70 mm.

[0065] After preparation is complete, close the vacuum chamber and evacuate to a vacuum level better than 8×10⁻⁶. -4 Pa;

[0066] Once the required vacuum level is reached, start the sample holder rotation, set the rotation speed of the sample holder to 5 r / min, and set the substrate temperature to 300℃.

[0067] After the substrate temperature reaches the set value, the argon gas flow rate is set to 70 sccm. The gas path valve is opened, and the regulating valve is used to adjust the working gas pressure in the vacuum coating chamber to 0.8 Pa. The DC power switch is turned on, and the current value of the TiNbMoTaCr composite target at target position 1 is adjusted to 0.3 A and the voltage value to 304 V; the current value of the MoS2 target at target position 2 is adjusted to 0.3 A and the voltage value to 533 V. After the glow discharge stabilizes, the target baffle control program is set. Target baffle 1 is opened so that target position 1 faces the substrate for 10 seconds, during which time target baffle 2 blocks target position 2. Then, target baffle 2 is opened so that target position 2 faces the substrate for 13 seconds, during which time target baffle 1 blocks target position 1. This cycle is repeated, with a cycle period of 66 times. After the cycle ends, the sample baffle is closed.

[0068] After deposition is complete, turn off the current to the TiNbMoTaCr composite target at target site 1 and the MoS2 target at target site 2, stop the argon gas supply, shut off the sample heating system, turn the modulation gate valve to its maximum, and wait for the sample heating temperature controller to display a temperature drop to room temperature before removing the sample. Then, alternately deposit the sample onto a titanium sheet to obtain l TiNbMoTaCr =10nm, l MoS2 =5nm TiNbMoTaCr / MoS2 nanolayer film; wherein l TiNbMoTaCr Represents the thickness of each TiNbMoTaCr nanolayer, l MoS2 This represents the thickness of each MoS2 nano-lubricant layer.

[0069] The l obtained in this embodiment MoS2 Friction experiments were conducted on a 5 nm TiNbMoTaCr / MoS2 nanolayer film. The friction coefficient curve and wear rate are shown below. Figure 2 As shown, its coefficient of friction is 0.4, and its wear rate is 1.414 × 10⁻⁶. -6 mm 3 / Nm. l MoS2 The stable friction coefficient curve of the 5nm TiNbMoTaCr / MoS2 nanomultilayer film indicates that the prepared multilayer film has excellent tribological properties of low friction and wear resistance.

[0070] Comparative Example 1

[0071] The titanium sheet was ultrasonically cleaned for 20 minutes in an ultrasonic cleaner with acetone and anhydrous ethanol respectively. The titanium sheet was then dried with dry nitrogen to obtain a clean substrate, which was then mounted on the substrate holder. The TiNbMoTaCr composite target was mounted on target position 1. The substrate holder was placed on the sample holder, and the target-substrate distance was adjusted to 70 mm.

[0072] After preparation is complete, close the vacuum chamber and evacuate to a vacuum level better than 8×10⁻⁶. -4 Pa;

[0073] Once the required vacuum level is reached, start the sample holder rotation, set the rotation speed of the sample holder to 5 r / min, and set the substrate temperature to 300℃.

[0074] After the substrate temperature reaches the set value, set the argon gas flow rate to 70 sccm, open the gas path valve, control the regulating valve to make the working gas pressure in the vacuum coating chamber 0.8 Pa, turn on the DC power switch, adjust the current value of TiNbMoTaCr composite target No. 1 to 0.3 A, and the voltage value to 304 V. After the glow discharge stabilizes, open the No. 1 target baffle so that the No. 1 target faces the substrate, set the sputtering time to 2 hours, and close the sample baffle and the No. 1 target baffle after sputtering is completed.

[0075] After deposition is complete, turn off the current to the TiNbMoTaCr composite target at target site 1, stop the argon gas supply, turn off the sample heating system, turn the modulation gate valve to the maximum, and wait for the sample heating temperature controller to show that the temperature has dropped to room temperature before taking out the sample and depositing TiNbMoTaCr films alternately on the titanium sheet.

[0076] Friction experiments were conducted on the TiNbMoTaCr film obtained in this comparative example, and the friction coefficient curve is shown below. Figure 2 As shown in the left figure, its coefficient of friction is very high and unstable, fluctuating in the range of approximately 0.6 to 0.8, resulting in severe wear.

[0077] Comparative Example 2

[0078] The titanium sheet was ultrasonically cleaned for 20 minutes each with acetone and anhydrous ethanol in an ultrasonic cleaner, and then dried with dry nitrogen to obtain a clean substrate, which was then mounted on the substrate holder. The MoS2 target was mounted at target position 2, the substrate holder was placed on the sample holder, and the target-substrate distance was adjusted to 70 mm.

[0079] After preparation is complete, close the vacuum chamber and evacuate to a vacuum level better than 8×10⁻⁶. -4 Pa;

[0080] Once the required vacuum level is reached, start the sample holder rotation, set the rotation speed of the sample holder to 5 r / min, and set the substrate temperature to 300℃.

[0081] After the substrate temperature reaches the set value, set the argon gas flow rate to 70 sccm, open the gas path valve, control the regulating valve to make the working gas pressure in the vacuum coating chamber 0.8 Pa, turn on the DC power switch, adjust the MoS2 target current value of target position 2 to 0.3 A, and the voltage value to 533 V. After the glow discharge stabilizes, open the target baffle of target position 2 so that target position 2 faces the substrate, set the sputtering time to 15 minutes, and close the sample baffle and target baffle of target position 2 after sputtering is completed.

[0082] After deposition is complete, turn off the current to the MoS2 target at target position 2, stop the argon gas supply, turn off the sample heating system, turn the modulation gate valve to the maximum, and wait for the sample heating temperature controller to show that the temperature has dropped to room temperature before taking out the sample and depositing MoS2 films alternately on the titanium sheet.

[0083] Friction experiments were conducted on the MoS2 film obtained in this comparative example. The friction coefficient curve and wear rate are shown below. Figure 2 As shown, its coefficient of friction gradually increases with time, and when the coefficient of friction is 0.2, its wear rate is 1.026 × 10⁻⁶. -6 mm 3 / Nm.

[0084] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film, comprising alternating layers of TiNbMoTaCr high-entropy alloy nanolayers and MoS2 nanolubricating layers; wherein the TiNbMoTaCr high-entropy alloy nanolayers have a hybrid structure of amorphous and nanocrystalline materials; wherein the MoS2 nanolubricating layers comprise bent MoS2 nanosheets; wherein the thickness of each TiNbMoTaCr high-entropy alloy nanolayer is 5-20 nm, and the thickness of each MoS2 nanolubricating layer is 5-10 nm; wherein the number of modulation units in the wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film is 40-80; and the thickness ratio of the TiNbMoTaCr high-entropy alloy nanolayer to the MoS2 nanolubricating layer within each modulation unit is independently 10:5-10.

2. The method for preparing the wear-resistant TiNbMoTaCr / MoS2 nanolayered film according to claim 1, comprising the following steps: A wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film was obtained by alternately sputtering the substrate with a TiNbMoTaCr composite target and a MoS2 target.

3. The preparation method according to claim 2, characterized in that, The TiNbMoTaCr composite target is composed of Ti target, Nb target, Mo target, Ta target and Cr target spliced ​​together.

4. The preparation method according to claim 3, characterized in that, The TiNbMoTaCr composite target uses a DC power supply; the sputtering current of the TiNbMoTaCr composite target is 0.2~0.4A; The distance between the TiNbMoTaCr composite target and the substrate is 60~80mm.

5. The preparation method according to claim 2, characterized in that, The MoS2 target uses a DC power supply or a radio frequency power supply.

6. The preparation method according to claim 5, characterized in that, When the MoS2 target uses a DC power supply, the DC sputtering current of the MoS2 target is 0.2~0.3A; when the MoS2 target uses an RF power supply, the RF sputtering power of the MoS2 target is 30~100W. The distance between the MoS2 target and the substrate is 60~80mm.

7. The preparation method according to claim 2, characterized in that, Before the alternating sputtering, the substrate temperature is set to 200~400℃.

8. The wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film of claim 1 or the wear-resistant TiNbMoTaCr / MoS2 nanomultilayer film prepared by any one of claims 2 to 7 as a protective coating.

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