AlTiMoVN multi-element self-lubricating coating as well as preparation method and application thereof

Abstract

The invention discloses an AlTiMoVN multi-element self-lubricating coating as well as a preparation method and application thereof. The preparation method comprises the following process steps: S1, ultrasonically cleaning a substrate; s2, the substrate is loaded to a sample holder and placed in a coating chamber, the temperature of the coating chamber is set to be 25-500 DEG C, and the vacuum degree of the coating chamber is set to be 1.0 * 10 <-3 >-1.0 * 10 <-4 > Pa; s3, inert gas and nitrogen are introduced into the coating chamber, the flow ratio of the inert gas to the nitrogen is 1: 1-5: 1, the vacuum degree is set to be 0.5-1.0 Pa, and the bias voltage is set to be 0-200 V; and S4, a high-power pulse magnetron sputtering power source is started, a target material is an AlTiMoV target, the power of the target material is set to be 1-9 kW, the duty ratio is set to be 10%-50%, and the deposition time is 60-180 min. The AlTiMoVN multi-element self-lubricating coating is obtained by deposition according to the preparation method disclosed by the invention. The AlTiMoVN multi-element self-lubricating coating can be applied to a cutter coating or a surface lubricating coating.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of surface engineering and coating technology, in particular to an AlTiMoVN multi-element self-lubricating coating, a preparation method and application thereof. BACKGROUND

[0002] In recent years, with the development of industrial manufacturing towards high efficiency, precision and green, the friction and wear scenarios such as cutting machining put forward higher requirements for coating materials. Although traditional liquid lubricants have significant effect in reducing friction, their volatile and leaky characteristics not only may pollute the environment, but also are difficult to be effectively applied in special working conditions such as high temperature, high speed or vacuum. Therefore, developing new type of dry solid lubricating coating materials with environmental protection, high efficiency and strong adaptability has become an important direction to improve the performance of cutting tools, molds and wear-resistant parts.

[0003] Among many hard coating materials, transition metal nitrides such as TiN and CrN are widely used due to their good hardness, wear resistance and chemical stability. However, these coatings usually exhibit high friction coefficient, and when working under no or little lubrication conditions, they still face serious wear problems, which limits their application in high-precision and long-life machining fields. In order to improve this situation, researchers are constantly exploring new coating systems with self-lubricating properties.

[0004] Researchers have found that introducing multiple elements into a single nitride matrix to form a multi-element alloyed coating can significantly optimize the comprehensive performance of the coating. For example, the incorporation of aluminum (Al) further improves the hardness of the coating due to solid solution strengthening, and a thin and dense Al2O3 film is formed on the surface at high temperature, effectively improving the oxidation resistance and high-temperature wear resistance of the coating. In addition, the introduction of lubricating phase elements such as molybdenum (Mo) or vanadium (V) not only helps to improve the hardness of the coating, but also the Mo-O or V-O oxide formed on the friction surface has good self-lubricating effect, effectively reducing the friction coefficient of the coating.

[0005] However, it should be noted that the oxide phases (such as Mo-O and V-O) in the coating that may play a lubricating role are often sensitive to temperature, with Mo-O performing better at medium and low temperatures (25 to 500℃), and V-O being more effective at high temperatures (500 to 800℃). Therefore, how to accurately control the ratio of each element and optimize the deposition process to obtain an AlTiMoVN coating with excellent wear resistance and wide temperature range self-lubricating properties is still a technical challenge currently faced by research and a key problem that the present application aims to solve. SUMMARY

[0006] To solve at least one of the above technical problems, the present application provides an AlTiMoVN multi-element self-lubricating coating, a preparation method and application thereof, and the technical solutions adopted are as follows.

[0007] The application provides a preparation method of an AlTiMoVN multi-element self-lubricating coating.

[0008] S1, ultrasonic cleaning of the substrate;

[0009] S2, loading the substrate into a sample holder and placing it into a coating chamber, setting the temperature of the coating chamber to 25-500 DEG C, and setting the vacuum degree to 1.0*10 -3 -1.0*10 -4 Pa;

[0010] S3, introducing inert gas and nitrogen into the coating chamber, the flow ratio of the inert gas and the nitrogen being 1:1-5:1, the vacuum degree being set to 0.5-1.0 Pa, and the bias voltage being set to 0 to-200 V;

[0011] S4, starting a high-power pulsed magnetron sputtering power source, the target material being an AlTiMoV target, the target material power being set to 1-9 kW, the duty cycle being set to 10%-50%, and the deposition time being 60-180 min.

[0012] In some embodiments of the application, the target material used in step S4 is a planar inlaid target, and the surface of the target material is inlaid with Ti targets, Al targets, Mo targets and V targets.

[0013] In some embodiments of the application, the number of Mo targets inlaid in different regions of the surface of the target material is different, and by adjusting the orientation of the substrate towards different regions or the different positions of the substrate loaded on the sample holder, an AlTiMoVN multi-element self-lubricating coating with different element contents can be obtained in step S4.

[0014] In some embodiments of the application, the target-substrate distance is set to 100-200 mm.

[0015] In some embodiments of the application, the substrate is high-speed steel or cemented carbide.

[0016] The AlTiMoVN multi-element self-lubricating coating provided by the application is deposited by using the preparation method described above.

[0017] In some embodiments of the application, the atomic percentage content of the elements in the AlTiMoVN multi-element self-lubricating coating is respectively Al: 20-35 at.%, Ti: 15-30 at.%, Mo: 0-15 at.%, V: 0-15 at.%, and N: 40-55 at.%.

[0018] In some embodiments of the application, the hardness of the AlTiMoVN multi-element self-lubricating coating is 30-40 GPa.

[0019] In some embodiments of the present application, the thickness of the AlTiMoVN multi-element self-lubricating coating is 1.0-3.0 μm.

[0020] The AlTiMoVN multi-element self-lubricating coating provided by the present application can be applied to a tool coating or a surface lubricating coating.

[0021] Compared with the prior art, the scheme of the present application has at least the following beneficial effects.

[0022] The AlTiMoVN multi-element self-lubricating coating utilizes the composite and synergistic effect of multi-element, not only maintains high hardness and excellent wear resistance of the coating, but also effectively promotes the formation of phases or structures capable of playing a lubricating role in different temperature ranges, thereby realizing wide-temperature-range self-lubrication and overcoming the temperature applicability limitation of a single lubricating phase.

[0023] On the basis of maintaining high hardness and wear resistance, the AlTiMoVN multi-element self-lubricating coating significantly reduces the friction coefficient, and realizes a good balance between wear resistance and self-lubrication.

[0024] The excellent self-lubricating performance of the AlTiMoVN multi-element self-lubricating coating can effectively reduce tool wear, reduce machining resistance, improve machining surface quality, or prolong the service life of precision mechanical parts, wear-resistant molds, etc.

[0025] Additional aspects and advantages of the present application will be in part apparent and in part pointed out hereinafter. BRIEF DESCRIPTION OF DRAWINGS

[0026] The present application will be further illustrated below in conjunction with the drawings and examples. It should be noted that the examples embodied in the following drawings are exemplary and are only used to explain the present application, and cannot be understood as a limitation on the present application.

[0027] Fig. 1 It is a schematic diagram of target material distribution for two planar mosaic target surfaces, and a schematic diagram of four positions of a corresponding sample holder.

[0028] Fig. 2 It is a SEM cross-sectional view of the coating in four examples, wherein (a) Mo: 0.3 at.%; (b) Mo: 3.3 at.%; (c) Mo: 6.8 at.%; (d) Mo: 8.9 at.%.

[0029] Fig. 3 It is a room temperature friction coefficient curve of the coating in four examples. DETAILED DESCRIPTION

[0030] The following will be described in conjunction with Figs. 1 to 3Detailed description of embodiments of the present application is made, wherein the same or similar reference signs represent the same or similar elements or elements having the same or similar functions throughout. The embodiments described below by referring to the drawings are exemplary and are only for the purpose of explaining the present application and cannot be understood as a limitation of the present application.

[0031] In the description of the present application, it is to be understood that the orientation or positional relationship indicated by the terms "center", "middle", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "axial", "radial", "circumferential" and the like are based on the orientation or positional relationship shown in the drawings, and are only for the purpose of facilitating the description of the present application and simplifying the description, and therefore cannot be understood as indicating or implying that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation of the present application.

[0032] In the description of the present application, if the meaning of several is more than one, the meaning of multiple is more than two, greater than, less than, more than, etc. are understood as not including the number, above, below, within, etc. are understood as including the number. If it is described that the first, the second is only for the purpose of distinguishing the technical features, and cannot be understood as indicating or implying the relative importance of the indicated technical features or implying the number of the indicated technical features or implying the sequence of the indicated technical features.

[0033] In the description of the present application, unless otherwise explicitly specified and limited, the terms "set", "mount", "connected", "connected" should be understood broadly, for example: it can be fixedly connected, or it can be detachably connected, or integrally connected; it can be mechanically connected, or it can be electrically connected; it can be directly connected, or it can be indirectly connected through an intermediate medium; it can be the communication inside two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0034] In the description of the present application, if the description of the terms "one embodiment", "some embodiments", "one example", "some examples", "some embodiments", "illustrative embodiments", "example", "specific example", "some examples" and the like means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present application. In the present specification, the illustrative description of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0035] The application relates to an AlTiMoVN multi-element self-lubricating coating, and the AlTiMoVN multi-element self-lubricating coating is obtained by high-power pulse magnetron sputtering deposition.

[0036] The atomic percentage content of elements in the AlTiMoVN multi-element self-lubricating coating is as follows: Al: 20-35 at.%, Ti: 15-30 at.%, Mo: 0-15 at.%, V: 0-15 at.%, and N: 40-55 at.%.

[0037] The application introduces or promotes the formation of phases or structures with self-lubricating functions by carefully designing the combination and proportion of Al, Ti, Mo, V and N elements and utilizing the synergistic effect among the elements, while maintaining high hardness and excellent wear resistance, wherein Mo-O and V-O are lubricating phases, so that the friction coefficient of the coating in the friction process is significantly reduced, the comprehensive tribological performance is improved, and the application potential under wide temperature conditions is improved.

[0038] The AlTiMoVN multi-element self-lubricating coating has a hardness of 30-40 Gpa and has high hardness characteristics, and the coating has good wear resistance, 10 -15 to 10 -16 m 3 / N.m.

[0039] The thickness of the AlTiMoVN multi-element self-lubricating coating is 1.0-3.0 mu m.

[0040] The AlTiMoVN multi-element self-lubricating coating has a columnar crystal structure.

[0041] The application relates to an application of an AlTiMoVN multi-element self-lubricating coating, and the AlTiMoVN multi-element self-lubricating coating can be applied to a tool coating or a surface lubricating coating, and is particularly suitable for working conditions sensitive to friction and wear and requiring a low friction coefficient, such as high-speed cutting tools, wear-resistant molds, precision mechanical parts and the like, so as to prolong the service life, improve the machining precision or operation efficiency.

[0042] The application relates to a preparation method of an AlTiMoVN multi-element self-lubricating coating, and the preparation method deposits the AlTiMoVN multi-element self-lubricating coating by a high-power pulse magnetron sputtering technology, optimizes deposition process parameters and controls a deposition rate, ensures that the coating obtains a target chemical composition and a microstructure, and realizes a good balance between wear resistance and self-lubricating property of the coating.

[0043] The preparation method comprises the following process steps.

[0044] S1, ultrasonic cleaning of a substrate;

[0045] S2, the substrate is loaded into the sample holder and placed in the coating chamber. The temperature of the coating chamber is set to 25 to 500°C, and the vacuum degree is set to 1.0*10. -3 Up to 1.0*10 -4 Pa;

[0046] S3, the coating chamber is purged with inert gas and nitrogen, the flow ratio of inert gas and nitrogen is 1:1 to 5:1, the vacuum degree is set to 0.5 to 1.0 Pa, and the bias voltage is set to 0 to -200 V;

[0047] S4, turn on the high-power pulsed magnetron sputtering power supply, the target material is an AlTiMoV target, the target power is set to 1 to 9 kW, the duty cycle is set to 10% to 50%, and the deposition time is 60 to 180 min.

[0048] Understandably, after the coating is completed, the high-power pulsed magnetron sputtering power supply, bias power supply, temperature control power supply and gas flow valve are turned off, and the furnace door is opened to remove the sample after the coating chamber cools down to room temperature.

[0049] It should be noted that in step S1, the substrate is made of high-speed steel or cemented carbide. After mirror polishing, the substrate is placed in an ultrasonic cleaner and ultrasonically cleaned with acetone and anhydrous ethanol for 10 to 20 minutes in sequence. After drying, it is fixed on the sample holder in the coating chamber.

[0050] The inert gas introduced into the coating chamber is argon.

[0051] During the deposition process, the target-substrate distance is set to 100 to 200 mm.

[0052] It should be noted that the target material used in step S4 is a planar inlaid target, with Ti, Al, Mo, and V targets inlaid on its surface. Furthermore, the number of Mo targets inlaid in different areas of the target surface varies. By adjusting the orientation of the substrate to different areas or by loading the substrate at different positions on the sample holder, step S4 can obtain AlTiMoVN multi-element self-lubricating coatings with different elemental contents.

[0053] In some examples, there are two planar inlay targets, and the surfaces of both targets are inlaid with Ti targets, Al targets, Mo targets and V targets, and the Ti targets, Al targets, Mo targets and V targets are all cylindrical targets.

[0054] Furthermore, the sample holder has four positions for loading the substrate. Position 1 corresponds to a planar mosaic target with 0 Mo targets embedded in the target area; position 2 corresponds to a planar mosaic target with 1 Mo target embedded in the target area; position 3 corresponds to a planar mosaic target with 2 Mo targets embedded in the target area; and position 4 corresponds to a planar mosaic target with 3 Mo targets embedded in the target area. In this case, by loading the substrate into position 1, 2, 3, or 4 of the sample holder, the composition content of the coating on the substrate can be controlled.

[0055] It should be noted that, compared with the prior art, the technical solution of this application has at least the following beneficial effects.

[0056] Multi-element synergy, wide temperature range self-lubrication: By utilizing the composite and synergistic effects of five elements, Al, Ti, Mo, V, and N, not only is the high hardness and excellent wear resistance of the coating maintained, but also the optimized ratio effectively promotes the formation of phases or structures that can play a lubricating role in different temperature ranges (such as the Mo-O phase at medium and low temperatures and the VO phase at high temperatures). This achieves effective self-lubrication over a wider temperature range, overcoming the problem of the limited temperature applicability of a single lubricating phase.

[0057] Balanced performance and excellent overall tribological properties: While ensuring high hardness and wear resistance, the coefficient of friction is significantly reduced, achieving a good balance between wear resistance and self-lubrication. This is due to the precise control of element ratios and optimized microstructure, which ensures the best match between the hard phase and the potential soft lubricating phase or structure, thus producing a self-lubricating coating with excellent overall tribological properties.

[0058] With broad application potential, the coating enhances service life and efficiency: its excellent self-lubricating properties effectively reduce tool wear, lower machining forces, improve the quality of machined surfaces, extend the service life of precision mechanical parts, wear-resistant molds, etc., and thus improve overall production efficiency.

[0059] The contents of this application are described in detail below with reference to specific embodiments. It should be noted that the following description is merely illustrative and not a specific limitation of this application.

[0060] Example 1

[0061] The preparation method includes the following process steps.

[0062] S1, the substrate after ultrasonic cleaning and mirror polishing.

[0063] S2, the substrate device is placed on the sample holder and then into the coating chamber. The target-substrate distance is 150 mm. The temperature of the coating chamber is set to 450℃, and the vacuum degree is set to 5.0*10. -3 Pa.

[0064] S3, Argon and nitrogen are introduced into the coating chamber, with an argon to nitrogen flow rate ratio of 3:1, a vacuum degree of 0.8 Pa, and a bias voltage of -120 V.

[0065] S4, turn on the high-power pulsed magnetron sputtering power supply, use a planar embedded target, the target composition is AlTiMoV, adjust the power to 6kW, adjust the duty cycle to 20%, and the deposition time to 120min.

[0066] The substrate is loaded at position 1 of the sample holder.

[0067] An AlTiMoVN multi-element self-lubricating coating with a thickness of 1.70 μm was deposited, and the atomic percentage contents of each element were Al: 30.5 at.%, Ti: 22.0 at.%, Mo: 0.3 at.%, V: 1.7 at.%, and N: 45.5 at.%.

[0068] Example 2

[0069] Compared to Example 1, the difference in Example 2 is that the substrate is loaded in position 2 of the sample holder.

[0070] An AlTiMoVN multi-element self-lubricating coating with a thickness of 1.75 μm was deposited, and the atomic percentage contents of each element were Al: 28.4 at.%, Ti: 22.6 at.%, Mo: 3.3 at.%, V: 1.5 at.%, and N: 44.2 at.%.

[0071] Example 3

[0072] Compared to Example 1, the difference in Example 3 is that the substrate is loaded in position 3 of the sample holder.

[0073] An AlTiMoVN multi-element self-lubricating coating with a thickness of 2.25 μm was deposited, and the atomic percentage contents of each element were Al: 24.7 at.%, Ti: 22.6 at.%, Mo: 6.8 at.%, V: 1.5 at.%, and N: 44.4 at.%.

[0074] Example 4

[0075] Compared to Example 1, the difference in Example 4 is that the substrate is loaded in position 4 of the sample holder.

[0076] An AlTiMoVN multi-element self-lubricating coating with a thickness of 2.37 μm was deposited, and the atomic percentage contents of each element were Al: 24.5 at.%, Ti: 21.3 at.%, Mo: 8.9 at.%, V: 1.2 at.%, and N: 44.1 at.%.

[0077] The coatings prepared in Examples 1 to 4 were subjected to structural characterization and performance testing.

[0078] Fig. 2 SEM cross-sectional images of the coatings with different Mo contents in the four embodiments are shown. Fig. 2 It can be seen that the coating exhibits a distinct columnar crystal structure, and the coating thickness gradually increases with the increase of Mo content.

[0079] Fig. 3 The coefficient of friction at room temperature is given for the coatings with different Mo contents in the four embodiments. Fig. 3 It can be seen that as the Mo content increases, the coefficient of friction of the coating gradually decreases.

[0080] The AlTiMoVN multi-element self-lubricating coating prepared in this application was deposited using high-power pulsed magnetron sputtering technology. Building upon traditional multi-element self-lubricating coatings, this method introduces and optimizes a composite system of key elements such as Al, Ti, Mo, V, and N, and controls the coating's proportions and microstructure. This effectively combines the synergistic strengthening effect among the multi-element components with a potential wide-temperature-range self-lubricating mechanism, ensuring that the coating achieves a significantly and stable low coefficient of friction while maintaining high hardness and excellent wear resistance. Therefore, the obtained coating exhibits superior and more balanced comprehensive tribological properties, providing a more efficient and reliable solution to friction and wear problems under complex working conditions (especially those with wide temperature variations).

[0081] The embodiments of this application have been described in detail above with reference to the accompanying drawings. However, this application is not limited to the above embodiments. Within the scope of knowledge possessed by those skilled in the art, various changes can be made without departing from the spirit of this application. Furthermore, unless otherwise specified, the embodiments and features described in the embodiments of this application can be combined with each other.

Claims

1. A method for preparing an AlTiMoVN multi-element self-lubricating coating, characterized in that: include S1, ultrasonic cleaning of the substrate; S2, the substrate is loaded into the sample holder and placed in the coating chamber. The temperature of the coating chamber is set to 25 to 500°C, and the vacuum degree is set to 1.0*10. -3 Up to 1.0*10 -4 Pa; S3, the coating chamber is purged with inert gas and nitrogen, the flow ratio of inert gas and nitrogen is 1:1 to 5:1, the vacuum degree is set to 0.5 to 1.0 Pa, and the bias voltage is set to 0 to -200 V; S4, turn on the high-power pulsed magnetron sputtering power supply, the target material is an AlTiMoV target, the target power is set to 1 to 9 kW, the duty cycle is set to 10% to 50%, and the deposition time is 60 to 180 min.

2. The method for preparing the AlTiMoVN multi-element self-lubricating coating according to claim 1, characterized in that: The target material used in step S4 is a planar inlaid target, and the surface of the target material is inlaid with Ti target, Al target, Mo target and V target.

3. The method for preparing the AlTiMoVN multi-element self-lubricating coating according to claim 1, characterized in that: The number of Mo targets embedded in different areas of the target surface varies. By adjusting the orientation of the substrate to different areas or by loading the substrate at different positions on the sample holder, step S4 can obtain AlTiMoVN multi-element self-lubricating coatings with different element contents.

4. The method for preparing the AlTiMoVN multi-element self-lubricating coating according to any one of claims 1 to 3, characterized in that: The target-base distance is set to 100 to 200 mm.

5. The method for preparing the AlTiMoVN multi-element self-lubricating coating according to any one of claims 1 to 3, characterized in that: The substrate is made of high-speed steel or hard alloy.

6. An AlTiMoVN multi-element self-lubricating coating, characterized in that: The AlTiMoVN multi-element self-lubricating coating is obtained by deposition using the preparation method described in any one of claims 1 to 5.

7. The AlTiMoVN multi-element self-lubricating coating according to claim 6, characterized in that: The atomic percentage contents of the elements in the AlTiMoVN multi-element self-lubricating coating are Al: 20 to 35 at.%, Ti: 15 to 30 at.%, Mo: 0 to 15 at.%, V: 0 to 15 at.%, and N: 40 to 55 at.%.

8. The AlTiMoVN multi-element self-lubricating coating according to claim 6, characterized in that: The hardness of the AlTiMoVN multi-element self-lubricating coating is 30 to 40 GPa.

9. The AlTiMoVN multi-element self-lubricating coating according to claim 6, characterized in that: The thickness of the AlTiMoVN multi-element self-lubricating coating is 1.0 to 3.0 μm.

10. An application of an AlTiMoVN multi-element self-lubricating coating, characterized in that: The AlTiMoVN multi-element self-lubricating coating as described in any one of claims 6 to 9 can be applied to tool coatings or surface lubrication coatings.

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