Metal disulfide composite film and preparation method and application thereof

Abstract

The invention provides a metal disulfide composite film and a preparation method and application thereof, and belongs to the technical field of composite films. The preparation method of the metal disulfide composite film provided by the invention comprises the following steps: mixing metal disulfide powder with a chelating agent, and carrying out cold press molding to obtain a composite molded body; the mass content of the chelating agent in the composite molding body is 0.1-10%; and by taking the composite forming body as a target material, depositing on the surface of a substrate by adopting a magnetron sputtering method to obtain the metal disulfide composite film. The metal disulfide composite film prepared by the method has excellent tribological performance in a vacuum environment, an atmospheric environment and a humid and hot environment, and is simple to operate and low in cost.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of composite film, in particular to a metal disulfide composite film and a preparation method and application thereof. BACKGROUND

[0002] With the rapid development of aerospace industry, the solid lubricating materials for aerospace represented by sputtered metal disulfide film such as sputtered MoS2 film, on the one hand, face more demanding service environments, such as high temperature, high humidity atmosphere on the ground, and extremely low temperature, high and low temperature alternation in orbit; on the other hand, long life and high precision aerospace moving parts put forward urgent demand for further greatly improving the tribological properties of lubricating materials. Therefore, carrying out the research on synergistically improving the environmental resistance and tribological properties of sputtered MoS2 film is not only conducive to improving the life and reliability of space moving mechanism, but also can further reduce the ground test and storage requirements, effectively reducing the storage and test cost of space moving mechanism.

[0003] At present, the method of element doping is often used to improve the tribological properties of sputtered MoS2 film, such as MoS2-Ti composite film obtained by doping Ti with MoS2 as matrix material. Although this method can improve the tribological properties of MoS2 film in vacuum environment, it will significantly reduce the tribological properties of MoS2 film in atmospheric environment and hot and humid environment. SUMMARY

[0004] The purpose of the present application is to provide a metal disulfide composite film and a preparation method and application thereof. The metal disulfide composite film prepared by the method of the present application has excellent tribological properties in vacuum environment, atmospheric environment and hot and humid environment, and is simple to operate and low in cost.

[0005] In order to achieve the above-mentioned purpose of the application, the present application provides the following technical scheme:

[0006] The present application provides a preparation method of a metal disulfide composite film, comprising the following steps:

[0007] Mixing metal disulfide powder and chelating agent, cold pressing to form a composite shaped body; the mass content of chelating agent in the composite shaped body is 0.1-10%;

[0008] Using the composite shaped body as target material, a metal disulfide composite film is deposited on the surface of the substrate by magnetron sputtering method.

[0009] Preferably, the chelating agent comprises hydroxyl carboxylic acid and / or hydroxyl carboxylic acid salt.

[0010] Preferably, the hydroxyl carboxylic acid comprises one or more of citric acid, lactic acid and tartaric acid, and the hydroxyl carboxylic acid salt comprises citrate.

[0011] Preferably, the citrate salt comprises one or more of trisodium citrate, disodium citrate and monosodium citrate.

[0012] Preferably, the metal disulfide powder comprises MoS2 powder and / or WS2 powder.

[0013] Preferably, the conditions of the magnetron sputtering method comprise: a vacuum chamber base vacuum degree less than 4.0*10-3Pa, a deposition gas pressure of 0.1-5.0 Pa, a deposition power of 100-600 W, and a negative bias voltage of 0--200 V. -3 Pa, a deposition gas pressure of 0.1-5.0 Pa, a deposition power of 100-600 W, and a negative bias voltage of 0--200 V.

[0014] Preferably, the working gas used for providing the deposition gas pressure is argon; and the material of the substrate comprises 9Cr18 steel, carbon steel or GCr15 steel.

[0015] The application provides a metal disulfide composite film prepared by the preparation method.

[0016] Preferably, the thickness of the metal disulfide composite film is 0.3-3 μm.

[0017] The application provides an application of the metal disulfide composite film as a solid lubricating material.

[0018] The application provides a preparation method of a metal disulfide composite film, which comprises the following steps: mixing metal disulfide powder and a chelating agent, and performing cold pressing to obtain a composite forming body; the mass content of the chelating agent in the composite forming body is 0.1-10%; and the composite forming body is used as a target material to deposit the metal disulfide composite film on a substrate surface by a magnetron sputtering method. The application utilizes the specific recognition of the chelating agent to the dangling bond of metal (such as molybdenum or tungsten) in the metal disulfide, and realizes high-efficiency passivation of the dangling bond in the film deposition process by using a co-sputtering technology, so that the metal disulfide composite film is finally prepared. The metal disulfide composite film has excellent tribological properties in a vacuum environment, an atmospheric environment and a hot and humid environment, has a wide application range, is simple to operate, low in cost, and suitable for large-scale production. BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 The infrared spectrum of the MoS2-0.4% C6H5Na3O7 composite film in Example 2 and the pure MoS2 film in Comparative Example 2;

[0020] Figure 2 The FESEM images of the MoS2-6% C6H5Na3O7 composite films prepared under different deposition gas pressures in Examples 3-4;

[0021] Figure 3 SEM images of wear tracks of MoS2-6% C6H5Na3O7 composite films prepared under different deposition pressures in Example 3-4 after friction in vacuum environment;

[0022] Figure 4 Friction curves of MoS2-6% C6H5Na3O7 composite films prepared under different deposition pressures in Example 3-4 in vacuum environment;

[0023] Figure 5 Friction curves of films prepared under different doping amounts of C6H5Na3O7 in Example 1-2 and Comparative Example 1-2 in vacuum environment;

[0024] Figure 6 Friction curves of films in Example 1-2 and Comparative Example 2 in natural environment;

[0025] Figure 7 Friction curves of films in Example 1-2 and Comparative Example 2 after storage in humid heat environment for 30 h in atmospheric environment;

[0026] Figure 8 Raman spectra of films in Example 1-2 and Comparative Example 2 after storage in humid heat environment for 30 h;

[0027] Figure 9 Friction curves of MoS2-Ti composite film in Comparative Example 3 in vacuum environment and natural environment, and friction curve of the film after storage in humid heat environment for 30 h in atmospheric environment. DETAILED DESCRIPTION

[0028] The present application provides a preparation method of metal disulfide composite film, comprising the following steps:

[0029] The metal disulfide powder is mixed with chelating agent, and cold-pressed to obtain a composite shaped body; the mass content of chelating agent in the composite shaped body is 0.1-10%;

[0030] The metal disulfide composite film is deposited on the surface of a substrate by using the composite shaped body as target material and adopting magnetron sputtering method.

[0031] In the present application, if no special description, the raw materials used are all commercially available goods known to those skilled in the art or prepared by methods known to those skilled in the art.

[0032] The metal disulfide powder is mixed with a chelating agent, and then cold-pressed to obtain a composite molding body. The chelating agent is used as a dangling bond passivation material, and can effectively passivate the dangling bonds of the metal disulfide composite film. The metal disulfide composite film obtained has excellent tribological properties in a vacuum environment, an atmospheric environment, and a humid and hot environment. In an embodiment of the present application, the chelating agent comprises a hydroxyl carboxylic acid and / or a hydroxyl carboxylic acid salt. The hydroxyl carboxylic acid can comprise one or more of citric acid, lactic acid, and tartaric acid. The hydroxyl carboxylic acid salt can comprise a citrate salt, which can be sodium citrate. The citrate salt can comprise one or more of trisodium citrate, disodium citrate, and monosodium citrate, and can specifically be trisodium citrate. In an embodiment of the present application, the metal disulfide powder can comprise MoS2 powder and / or WS2 powder, and can specifically be MoS2 powder. The conditions for cold-pressing are not particularly limited, and can be determined by those skilled in the art to ensure that the subsequent magnetron sputtering method can be met. The mass content of the chelating agent in the composite molding body is 0.1-10%, and can specifically be 0.1%, 0.4%, 0.8%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, or 10%. Limiting the mass content of the chelating agent to the above range is beneficial to obtaining a metal disulfide composite film with good tribological properties. If the mass content of the chelating agent is too high, the tribological properties of the metal disulfide composite film may be reduced.

[0033] After obtaining the composite molding body, the metal disulfide composite film is deposited on the surface of a substrate by a magnetron sputtering method using the composite molding body as a target. In an embodiment of the present application, the substrate can be made of a metal material, and the material of the substrate can comprise 9Cr18 steel, carbon steel, or GCr15 steel, and can specifically be 9Cr18 steel. In the embodiment of the present application, a workpiece on which the metal disulfide composite film is to be deposited is used as the substrate. In an embodiment of the present application, the substrate is preferably polished, polished, cleaned, and dried in sequence before use. The polishing and polishing are not particularly limited, and the substrate can be mirror finished. The cleaning can be ultrasonic cleaning, and the reagent used for ultrasonic cleaning can be an organic solvent, which can comprise one or more of ethanol, acetone, and petroleum ether. The ethanol can be anhydrous ethanol. In the embodiment of the present application, anhydrous ethanol and acetone are used for ultrasonic cleaning in sequence. The time for ultrasonic cleaning using each reagent can be ≥30 min, and can specifically be 30-40 min. The drying can be drying.

[0034] In an embodiment of the present application, the conditions of the magnetron sputtering method can comprise: the vacuum chamber background vacuum degree can be less than 4.0×10 -3Pa, and specifically can be less than 1.0*10 -3 Pa; the deposition gas pressure can be 0.1-5.0 Pa, and specifically can be 0.1 Pa, 0.5 Pa, 1.0 Pa, 1.5 Pa, 2.0 Pa, 2.5 Pa, 3.0 Pa, 3.5 Pa, 4.0 Pa, 4.5 Pa or 5.0 Pa; the working gas used to provide the deposition gas pressure can be argon; the deposition power can be 100-600 W, and specifically can be 100 W, 110 W, 120 W, 130 W, 140 W, 150 W, 180 W, 200 W, 300 W, 400 W, 500 W or 600 W; the negative bias voltage is 0--200 V, and further can be -10--100 V, and further can be -20--50 V, and specifically can be -35 V; the deposition time is based on ensuring that the metal disulfide composite film of desired thickness is obtained, and for example, the deposition time can be 10-120 min, and further can be 30-60 min, and specifically can be 40 min. In the embodiments of the present application, the equipment used in the magnetron sputtering method is a TWJY-CK-CQ high vacuum single-chamber three-target magnetron sputtering thin film deposition system.

[0035] The method of the present application can significantly improve the moisture and heat environment resistance of the metal disulfide composite film, and the metal disulfide composite film can still maintain excellent tribological properties in a moisture and heat environment. Specifically, by introducing a chelating agent as a dangling bond passivation material in the co-sputtering process, the present application can passivate the edge dangling bonds of the metal disulfide composite film in situ during the growth of the metal disulfide composite film, thereby improving the environmental resistance of the metal disulfide composite film; at the same time, by adjusting the conditions of the magnetron sputtering method, the compactness of the metal disulfide composite film can be increased, and the wear life of the metal disulfide composite film is also increased. In addition, by adjusting the conditions of the magnetron sputtering method such as the deposition gas pressure, the lubrication state of the chelating agent at the friction interface can be adjusted, thereby realizing the adjustment of the tribological properties of the metal disulfide composite film.

[0036] The metal disulfide composite film prepared by the preparation method of the technical scheme is provided, which comprises a metal disulfide base and a chelating agent doped in the metal disulfide base. As an embodiment of the present application, the thickness of the metal disulfide composite film can be 0.3-3 μm, and specifically can be 0.3 μm, 0.5 μm, 1 μm, 1.5 μm, 2 μm, 2.5 μm or 3 μm. As an embodiment of the present application, the metal disulfide composite film can be a porous film or a dense film, and the film density can be controlled by controlling the conditions of the magnetron sputtering method. For example, when the deposition power is 100 W and the deposition time is 40 min, the metal disulfide composite film obtained under the condition of a deposition gas pressure of 1.0 Pa is a porous film, and increasing the deposition gas pressure can make the metal disulfide composite film more dense. The chelating agent (such as trisodium citrate) in the metal disulfide composite film prepared by the method of the present application can still retain the original hydroxyl and carboxyl functional groups, but part of it also reacts to form NaOH and Na2O.

[0037] The application provides the application of the metal disulfide composite film as a solid lubricating material. As an embodiment of the present application, the solid lubricating material can be a solid lubricating material for aerospace. The metal disulfide composite film has excellent tribological properties in a vacuum environment, an atmospheric environment and a hot and humid environment, and can meet the harsh service environment. As an embodiment of the present application, the vacuum environment specifically refers to a vacuum degree less than 10 - 3 Pa; the atmospheric environment refers to a natural environment in an air atmosphere, and in the examples, the tribological properties of the metal disulfide composite film are tested in an air atmosphere with a temperature of 19 ℃ and a relative humidity of 17%; the hot and humid environment refers to a hot and humid environment in an air atmosphere, and in the examples, the tribological properties of the metal disulfide composite film are tested in the above-mentioned atmospheric environment after being stored in a hot and humid chamber (air atmosphere) with a temperature of 30 ℃ and a relative humidity of 90% for 30 h.

[0038] The technical solutions in the present application will be described clearly and completely in combination with the examples in the present application. Obviously, the described examples are only a part of the examples of the present application, rather than all the examples. Based on the examples in the present application, all the other examples obtained by a person of ordinary skill in the art without creative labor fall within the protection scope of the present application.

[0039] In the following experiments, all the reagents are analytical pure, and trisodium citrate (C6H5Na3O7) is purchased from Tianjin Fuchen Chemical Reagent Co., Ltd.; MoS2 powder (purity of 99.99%) is purchased from Beijing Guitian Yinchuang Technology Co., Ltd.

[0040] The equipment used in the following experiment is a TWJY-CK-CQ high vacuum single-chamber three-target magnetron sputtering thin film deposition system.

[0041] Example 1

[0042] 4 g of C6H5Na3O7 was uniformly mixed with 96 g of MoS2 powder, and cold-pressed to form a composite shaped body;

[0043] The surface of the workpiece (material: 9Cr18 steel) was polished to a mirror surface, and then ultrasonically cleaned in anhydrous ethanol and acetone for 30 min, respectively, and dried for standby use; the composite shaped body was used as a target material, and a MoS2-4% C6H5Na3O7 composite thin film was deposited on the surface of the dried workpiece by a magnetron sputtering method; the conditions of the magnetron sputtering method included: the vacuum chamber base vacuum degree was less than 1.0 x 10 -3 Pa, the deposition gas pressure was 3.0 Pa (the working gas used was argon), the deposition power (radio frequency power) was 100 W, the negative bias voltage was -35 V, and the deposition time was 40 min; after the deposition was completed, the workpiece was naturally cooled to room temperature and taken out, and the thickness of the MoS2-4% C6H5Na3O7 composite thin film was 2 μm.

[0044] Example 2

[0045] The method operation of Reference Example 1 was referred to, except that the preparation raw material of the composite shaped body was 0.4 g of C6H5Na3O7 and 99.6 g of MoS2 powder, and finally a MoS2-0.4% C6H5Na3O7 composite thin film was prepared by a magnetron sputtering method.

[0046] Example 3

[0047] The method operation of Reference Example 1 was referred to, except that the preparation raw material of the composite shaped body was 6 g of C6H5Na3O7 and 94 g of MoS2 powder, and finally a MoS2-6% C6H5Na3O7 composite thin film was prepared by a magnetron sputtering method.

[0048] Example 4

[0049] The method operation of Reference Example 3 was referred to, except that the deposition gas pressure was adjusted to 1.0 Pa, 2.0 Pa, 4.0 Pa or 5.0 Pa, respectively.

[0050] Comparative Example 1

[0051] The method operation of Reference Example 1 was referred to, except that the preparation raw material of the composite shaped body was 16 g of C6H5Na3O7 and 84 g of MoS2 powder, and finally a MoS2-16% C6H5Na3O7 composite thin film was prepared by a magnetron sputtering method.

[0052] Comparative Example 2

[0053] The method of Example 1 was operated with the difference that C6H5Na3O7 was omitted, i.e. the MoS2 powder was directly cold-pressed into a shape, and then a pure MoS2 film was prepared by magnetron sputtering.

[0054] Comparative Example 3

[0055] MoS2 powder was cold-pressed into a shape to obtain a MoS2 shaped body;

[0056] The surface of a workpiece (9Cr18 steel) was polished to a mirror surface, and then ultrasonically cleaned in anhydrous ethanol and acetone for 30 min, respectively, and dried for use. The MoS2 shaped body was used as a target material, and a metal Ti target material was used to co-deposit a MoS2-Ti composite film on the surface of the dried workpiece by magnetron sputtering. The conditions of the magnetron sputtering method included: the base vacuum degree of the vacuum chamber was less than 1.0 x 10 -3 Pa, the deposition gas pressure was 3.0 Pa (the working gas used was argon), the MoS2 deposition power (radio frequency power) was 100 W, the Ti deposition power was 30 W, the negative bias voltage was -35 V, and the deposition time was 40 min. After the deposition was completed, the workpiece was naturally cooled to room temperature and removed, and the thickness of the MoS2-Ti composite film was 2 μm.

[0057] Characterization and performance testing

[0058] Figure 1 The infrared spectra of the MoS2-0.4% C6H5Na3O7 composite film in Example 2 and the pure MoS2 film in Comparative Example 2 were compared. The results showed that in the infrared spectrum of the MoS2-0.4% C6H5Na3O7 composite film, the symmetric stretching vibration absorption peak and the asymmetric stretching vibration absorption peak of the carboxylate (-COO -1 ) were detected at 1410.68 cm -1 and 1594.50 cm - , respectively, and the associated state hydroxyl (O-H) stretching vibration peak was detected at 3259.90 cm -1 . This indicated that the hydroxyl and carboxylate groups in C6H5Na3O7 could be partially preserved.

[0059] Figure 2FESEM images of MoS2-6% C6H5Na3O7 composite films prepared in Example 3-4 under different deposition pressures, wherein a and b are surface FESEM images and cross-sectional FESEM images of the composite films under a deposition pressure of 1.0 Pa, c and d are surface FESEM images and cross-sectional FESEM images of the composite films under a deposition pressure of 3.0 Pa, e and f are surface FESEM images and cross-sectional FESEM images of the composite films under a deposition pressure of 4.0 Pa, and g and h are surface FESEM images and cross-sectional FESEM images of the composite films under a deposition pressure of 5.0 Pa. The results show that, under the same deposition time, increasing the deposition pressure within a certain range can make the composite film more compact when the deposition power is 100 W.

[0060] Figure 3 SEM images of wear tracks of MoS2-6% C6H5Na3O7 composite films prepared in Example 3-4 under different deposition pressures after friction in a vacuum environment, wherein the lower part is an enlarged view of the upper part; Figure 3 The conditions of the friction experiment involved in the application include a load of 5 N, a rotation speed of 1000 r / min, and a vacuum degree of less than 10 -3 Pa. The results show that, by adjusting the conditions of the magnetron sputtering method, the lubrication state of the chelating agent and MoS2 at the friction interface can be adjusted, wherein the chelating agent and MoS2 at the friction interface are rod-shaped rolling friction when the deposition pressure is 2.0 Pa, the chelating agent and MoS2 at the friction interface are spherical rolling friction when the deposition pressure is 3.0 Pa, and the chelating agent and MoS2 at the friction interface are sheet-shaped friction when the deposition pressure is 4.0 Pa, which shows that the method can be used to adjust the tribological properties of the metal disulfide composite film.

[0061] The friction coefficient and wear life data of the films in Example 1-4 and Comparative Example 1-2 in a vacuum environment are shown in Table 1; Figure 4 Friction curves of MoS2-6% C6H5Na3O7 composite films prepared in Example 3-4 under different deposition pressures in a vacuum environment, Figure 5 Friction curves of the films prepared in Example 1-2 and Comparative Example 1-2 under different doping amounts of C6H5Na3O7 in a vacuum environment; Table 1, Figure 4 and Figure 5 The conditions of the friction experiment involved in the application include a load of 5 N, a rotation speed of 1000 r / min, and a vacuum degree of less than 10 -3 Pa. From the Figure 4and Table 1, with the increase of the deposition pressure, the wear life of the composite film presents the trend of first increasing and then decreasing, and the friction coefficient also obviously decreases; wherein the deposition power is 100 W and the deposition pressure is 3.0 Pa or 4.0 Pa, the film obtained has relatively excellent friction coefficient and wear life. Figure 5 and Table 1, compared with the pure MoS2 film, the film with the C6H5Na3O7 doping amount of 0.4% or 4% has relatively long wear life, wherein the wear life of the MoS2-0.4%C6H5Na3O7 composite film is 5 times of that of the pure MoS2 film; compared with the pure MoS2 film, the tribological properties (friction coefficient, wear life) of the MoS2-16%C6H5Na3O7 composite film are significantly reduced, that is, too much C6H5Na3O7 doping amount will reduce the tribological properties of the film. The above results show that the composite film prepared in the embodiment of the application has excellent tribological properties in the vacuum environment.

[0062] Table 1, the friction coefficient and wear life of each film in the vacuum environment

[0063]

[0064] The friction coefficient and wear life data of the films in Examples 1-2 and Comparative Example 2 in the natural environment are listed in Table 2, Figure 6 is the friction curve of the film in Examples 1-2 and Comparative Example 2 in the natural environment; Table 2 and Figure 6 The conditions of the friction experiment involved include: air atmosphere, temperature of 19℃, relative humidity of 17%, load of 5N, and rotation speed of 1000 rpm. The results show that compared with the pure MoS2 film, the film with the C6H5Na3O7 doping amount of 0.4% or 4% has excellent tribological properties.

[0065] Table 2, the friction coefficient and wear life of each film in the natural environment

[0066] Sample origin Sample type Average coefficient of friction Wear life (r) Example 1 MoS2-4% C6H5Na3O7 composite film 0.058 2.6 x 10 5 ]]> Example 2 MoS2-0.4% C6H5Na3O7 composite thin film 0.041 1.2 x 10 6 ]]> Comparative Example 2 pure MoS2 film 0.120 3.0 x 10 4 ]]

[0067] The friction coefficient and wear life data of the films in Examples 1-2 and Comparative Example 2 after the treatment in the humid heat environment are listed in Table 3, Figure 7 is the friction curve of the film in Examples 1-2 and Comparative Example 2 in the humid heat environment; Table 3 and Figure 7The conditions involved in the friction experiment include: placing the sample in a humidity oven, which is an air atmosphere, the temperature is 30°C, and the relative humidity is 90%; after storing in the humidity oven for 30h, the sample is taken out and subjected to friction experiment in the natural environment (air atmosphere, temperature is 19°C, relative humidity is 17%), the load is 5N, and the rotation speed is 1000rpm. The results show that the friction coefficients of the pure MoS2 film and the MoS2-4% C6H5Na3O7 composite film after the treatment in the humid heat environment fluctuate obviously, and the wear life is 2.0x10 5 r and 1.4x10 5 r respectively, but the MoS2-0.4% C6H5Na3O7 composite film still maintains a low friction coefficient (specifically 0.040) and an ultra-long wear life (specifically 8.9x10 5 r).

[0068] Table 3 Friction coefficient and wear life of each film after treatment in the humid heat environment

[0069] Sample origin Sample type Coefficient of friction Wear life (r) Example 1 MoS2-4% C6H5Na3O7 composite film 0.080 1.4 x 10 5 ]]> Example 2 MoS2-0.4% C6H5Na3O7 composite thin film 0.040 8.9 x 10 5 ]]> Comparative Example 2 pure MoS2 film 0.059 2.0 x 10 5 ]]>

[0070] Figure 8 The Raman spectra of the films in Examples 1-2 and Comparative Example 2 after storing in the humid heat environment (air atmosphere, temperature is 30°C, relative humidity is 90%) for 30h are shown, specifically, the films are stored in the humid heat environment for 30h, and then the Raman spectra are obtained by using a Raman spectrometer. The results show that after storing in the humid heat environment for 30h, the pure MoS2 film surface has no obvious MoS2 characteristic peaks, but new characteristic peaks of molybdate compounds are generated. For the MoS2-4% C6H5Na3O7 composite film and the MoS2-0.4% C6H5Na3O7 composite film, two characteristic peaks of MoS2 are presented at 370cm -1 and 408cm -1 after storing in the humid heat environment for 30h; in addition, there is a Mo-O vibration peak characteristic peak at 920cm -1 . Therefore, C6H5Na3O7 passivates the dangling bonds by co-deposition, so that the obtained film has excellent anti-humid heat performance.

[0071] Figure 9 The friction curves of the MoS2-Ti composite film in Comparative Example 3 in the vacuum environment and the natural environment, and the friction curve in the atmospheric environment after storing in the humid heat environment for 30h are shown; Figure 9 The friction experiment conditions in different environments are consistent with Figure 5 , Figure 6 and Figure 7 . The results show that the wear life of the MoS2-Ti composite film in the vacuum environment, the natural environment and the humid heat environment is 1.3x105 r, 2.7 x 10 4 r, 4.0 x 10 3 r, the average friction coefficients are 0.027, 0.132 and 0.190 respectively. It is shown that the introduction of Ti can improve the tribological performance of the MoS2 film in vacuum, but the tribological performance of the MoS2 film in natural environment and humid heat environment is significantly decreased.

[0072] The above results show that the metal disulfide composite film prepared by the embodiment of the present application has excellent tribological performance in vacuum environment, atmospheric environment and humid heat environment, has wide application range, is simple to operate, low in cost and suitable for large-scale production.

[0073] The above only describes the preferred embodiments of the present application, and it should be noted that the ordinary skilled in the art can make several improvements and refinements without departing from the principles of the present application, and these improvements and refinements should also be considered as the protection scope of the present application.

Claims

1. A method for producing a metal disulfide composite film, characterized by, The method comprises the following steps: mixing metal disulfide powder with chelating agent, cold-pressing to obtain a composite molding body; the mass content of the chelating agent in the composite molding body is 0.1-10%; using the composite molding body as a target material, depositing a metal disulfide composite film on a substrate surface by a magnetron sputtering method.

2. The production method according to claim 1, characterized by, The chelating agent comprises hydroxyl carboxylic acid and / or hydroxyl carboxylic acid salt.

3. The production method according to claim 2, characterized by, The hydroxyl carboxylic acid comprises one or more of citric acid, lactic acid and tartaric acid, and the hydroxyl carboxylic acid salt comprises citrate.

4. The production method according to claim 3, characterized by, The citrate comprises one or more of trisodium citrate, disodium citrate and monosodium citrate.

5. The process according to any one of claims 1 to 4, characterized in that, The metal disulfide powder comprises MoS2 powder and / or WS2 powder.

6. The method of claim 1, wherein, The conditions of the magnetron sputtering method include: the base vacuum degree of a vacuum chamber is less than 4.0*10 -3 Pa, the deposition pressure is 0.1-5.0 Pa, the deposition power is 100-600 W, and the negative bias is 0--200 V.

7. The preparation method according to claim 6, characterized in that, The working gas used for the deposition gas pressure is argon, and the material of the substrate comprises 9Cr18 steel, carbon steel or GCr15 steel.

8. The metal disulfide composite film prepared by the method according to any one of claims 1 to 7, characterized in that, The metal disulfide composite film comprises a metal disulfide base and a chelating agent doped in the metal disulfide base.

9. The metal-disulfide composite film of claim 8, wherein, The thickness of the metal disulfide composite film is 0.3-3 μm.

10. Use of the metal disulfide composite film according to claim 8 or 9 as a solid lubricant.

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