Self-lubricating composite coating, method for preparing same and use thereof

Abstract

The present application relates to a kind of self-lubricating composite coating and its preparation method and application, the self-lubricating composite coating includes at least 1 layer composite structure;The composite structure includes the AlTiX a N layer and W 1‑m Me m N layer.The self-lubricating composite coating provided by the present application controls diffusion process by the synergistic cooperation of AlTiX a N layer and W 1‑m Me m N layer, inhibits the rapid oxidation of lubricating component, reduces wear rate, can obtain the coating of low friction coefficient and low wear rate, therefore, self-lubricating composite coating can be widely used in metal surface treatment or metal processing.

Description

Technical Field

[0001] This invention belongs to the field of materials technology, and relates to a coating material, and more particularly to a self-lubricating composite coating and its preparation method and application. Background Technology

[0002] Aluminum nitride coatings are currently the mainstream tool coatings. Solid solutions and cubic AlTiN (c-TiAlN) have become a research hotspot for high-speed, dry machining tool coatings due to their excellent mechanical properties, high-temperature stability, and wear resistance. However, c-AlTiN coatings, which perform well in high-speed milling under high-temperature service environments, still have some problems. For example, the coating undergoes amplitude modulation decomposition at temperatures of 750℃-850℃. If the temperature continues to rise, w-AlN (wurtzite-AlN) will precipitate from the coating, leading to a decrease in mechanical properties. AlTiN coatings have a high coefficient of friction at high temperatures, which can easily lead to problems such as high cutting forces, chatter, and severe wear on the tool. The oxidation initiation temperature is relatively low. During machining, the coating is preferentially oxidized before it has undergone amplitude modulation decomposition and hardening, making it difficult to adapt to dry machining of materials such as titanium alloys and high-temperature alloys. When using AlTiN coated tools for dry machining, the coating is prone to adhesion and diffusion with the workpiece, resulting in a decrease in tool life. Therefore, further improving the high-temperature oxidation resistance, high-temperature mechanical and phase structure stability, and high-temperature wear and friction reduction properties of AlTiN coatings has important theoretical significance and practical application value for promoting the development of coated cutting tools and the metal processing industry.

[0003] Currently, common methods include optimizing the elemental composition of hard coatings to generate Magnéli phase solid oxides with high ionic potential on their surface under high-temperature conditions. The high-temperature self-lubricating properties of these solid oxides are then utilized to reduce the coefficient of friction of the coating under high-temperature conditions. For example, V in AlTiVN coatings can rapidly diffuse to the coating surface at high temperatures and oxidize to form the lubricant V₂O₅, thus reducing the coefficient of friction. However, V readily undergoes rapid outward diffusion along columnar grain boundaries, causing a sharp decrease in the oxidation initiation temperature of the AlTiVN coating. Furthermore, the resulting V₂O₅ has a loose structure, poor mechanical properties, and is easily worn, ultimately leading to a low coefficient of friction and high wear rate in AlTiVN coatings under high-temperature service conditions, failing to meet the performance requirements of tool coatings for difficult-to-machine materials. Therefore, improving the high-temperature self-lubricating properties of AlTiN coatings while simultaneously reducing the diffusion rate of self-lubricating components under high-temperature service conditions, thereby avoiding damage to the coating's resistance to high-temperature oxidation, is a key issue in achieving wear resistance and friction reduction in coatings at high temperatures.

[0004] Therefore, there is a need to provide a self-lubricating composite coating with low friction coefficient and low wear rate at higher temperatures, as well as its preparation method and application. Summary of the Invention

[0005] To address the shortcomings of existing technologies, the present invention aims to provide a self-lubricating composite coating, its preparation method, and its application. The self-lubricating composite coating utilizes AlTiX... a N-layer and W 1-m Me m The synergistic effect of the N-layer controls the diffusion process, inhibits the rapid oxidation of lubricating components, and reduces the wear rate, resulting in a coating with low friction coefficient and low wear rate. Therefore, self-lubricating composite coatings can be widely used in metal surface treatment or metal processing.

[0006] To achieve this objective, the present invention adopts the following technical solution:

[0007] In a first aspect, the present invention provides a self-lubricating composite coating, the self-lubricating composite coating comprising at least one composite structure.

[0008] The composite structure includes stacked AlTiX a N-layer and W 1-m Me m N layers.

[0009] The AlTiX a In layer N, X is any one or a combination of at least two of Ti, Cr, Zr, Ta, Hf, Y, Nb, Sc, Mo, V, W, Si, O, or B, and a ≤ 0.2.

[0010] The W 1-m Me m In layer N, m≤0.5, and Me is any one or at least two of Zr, Ta, Hf, Y, Nb, Sc, Mo, W or V.

[0011] The self-lubricating composite coating provided by this invention utilizes AlTiX a N-layer and W 1-m Me m The synergistic effect of the N-layer controls the diffusion process, inhibits the rapid oxidation of lubricating components, and reduces the wear rate, resulting in a coating with low friction coefficient and low wear rate. Therefore, self-lubricating composite coatings can be widely used in metal surface treatment or metal processing.

[0012] Preferably, in the composite structure, AlTiX a The thickness of the N layer is ≤5μm.

[0013] Preferably, in the composite structure, W 1-m Me m The thickness of the N layer is ≤5μm.

[0014] Preferably, the hardness of the self-lubricating composite coating is 18.8 GPa-38.8 GPa.

[0015] Preferably, the elastic modulus of the self-lubricating composite coating is 406 GPa-505 GPa.

[0016] Preferably, the self-lubricating composite coating has a room temperature (25°C) friction coefficient of 0.32-0.61 and a high temperature (500°C) friction coefficient of 0.29-0.35.

[0017] Preferably, the self-lubricating composite coating has a room temperature (25°C) wear rate of 0.52 × 10⁻⁶. -7 mm 3 / (N·m)-5.06×10 -7 mm 3 / (N·m), the high-temperature (500℃) wear rate is 12.3×10 -7 mm 3 / (N·m)-77.8×10 -7 mm 3 / (N·m).

[0018] Secondly, the present invention provides a method for preparing a self-lubricating composite coating, the method comprising the following steps:

[0019] AlTiX was alternately sputtered by magnetron sputtering in a nitrogen-containing mixed atmosphere. a Target material and W 1-m Me m The target material is deposited on the substrate surface to obtain the self-lubricating composite coating described in the first aspect.

[0020] The AlTiX a X in the target material is any one or a combination of at least two of Ti, Cr, Zr, Ta, Hf, Y, Nb, Sc, Mo, V, W, Si, O or B, and a≤0.2.

[0021] The W 1-m Me m In the target material, m≤0.5, and Me is any one or a combination of at least two of Zr, Ta, Hf, Y, Nb, Sc, Mo, W or V.

[0022] The preparation method provided by this invention uses magnetron sputtering to prepare AlTiX. a N-layer and W 1-m Me m Compared to traditional arc evaporation, magnetron sputtering can deposit densely packed, smooth, and high-density thin films on the substrate surface. Moreover, the resulting films have good thickness and composition uniformity, which helps to reduce the friction coefficient and wear rate of the resulting self-lubricating composite coating.

[0023] Preferably, the gas in the nitrogen-containing mixed atmosphere includes nitrogen and a balance gas.

[0024] Preferably, the balancing gas includes any one or a combination of at least two of helium, neon, argon, or krypton.

[0025] Preferably, during magnetron sputtering, the flow rate of N2 is ≤80 sccm.

[0026] Preferably, during magnetron sputtering, the substrate revolves at a speed of 0.5 rpm to 10 rpm.

[0027] Preferably, during magnetron sputtering, the bias voltage of the substrate is -50V to -500V.

[0028] Preferably, the deposition temperature during magnetron sputtering is between 150°C and 450°C.

[0029] Preferably, the absolute pressure during magnetron sputtering is 0.2 Pa to 0.8 Pa.

[0030] Preferably, the AlTiX is sputtered by magnetron sputtering. a Methods for using targets include DC magnetron sputtering or high-power pulsed magnetron sputtering.

[0031] Preferably, the W is magnetron sputtered 1-m Me m Methods for sputtering targets include DC magnetron sputtering, intermediate frequency magnetron sputtering, radio frequency magnetron sputtering, or high-power pulsed magnetron sputtering.

[0032] Preferably, the AlTiX a The magnetron sputtering power of the target is 5W / cm. 2 -20W / cm 2 .

[0033] Preferably, the AlTiX is sputtered using high-power pulsed magnetron sputtering. a The peak current density of the target material is 0.2 A / cm². 2 -1A / cm 2 .

[0034] Preferably, the W is subjected to high-power pulsed magnetron sputtering. 1-m Me m The peak current density of the target material is 0.2 A / cm². 2 -0.8A / cm 2 .

[0035] Thirdly, the present invention provides a cutting tool, the cutting tool comprising a tool body and a self-lubricating composite coating disposed on the tool body as described in the first aspect.

[0036] The numerical range described in this invention includes not only the point values ​​listed above, but also any point values ​​within the numerical ranges not listed above. Due to space limitations and for the sake of brevity, this invention will not exhaustively list all the specific point values ​​included in the range.

[0037] Compared with the prior art, the present invention has the following beneficial effects:

[0038] (1) The self-lubricating composite coating provided by this invention is made of AlTiX a N-layer and W 1-m Me m The synergistic effect of the N-layer controls the diffusion process, inhibits the rapid oxidation of lubricating components, and reduces the wear rate, resulting in a coating with low friction coefficient and low wear rate. Therefore, self-lubricating composite coatings can be widely used in metal surface treatment or metal processing.

[0039] (2) The preparation method provided by the present invention uses magnetron sputtering to prepare AlTiX a N-layer and W 1-m Me m Compared to traditional arc evaporation, magnetron sputtering can deposit densely packed and highly compact films on the substrate surface, and the resulting films have good thickness and composition uniformity, which is beneficial for reducing the friction coefficient and wear rate of the resulting self-lubricating composite coating. Attached Figure Description

[0040] Figure 1 These are the XRD patterns of the coatings obtained in Examples 1-5 and Comparative Example 1.

[0041] Figure 2 The image shows the cross-sectional SEM morphology of the self-lubricating coating obtained in Example 1.

[0042] Figure 3 The image shows the cross-sectional SEM morphology of the self-lubricating coating obtained in Example 2.

[0043] Figure 4 This is a cross-sectional SEM image of the self-lubricating coating obtained in Example 3.

[0044] Figure 5 This is a cross-sectional SEM image of the self-lubricating coating obtained in Example 4.

[0045] Figure 6 This is a cross-sectional SEM image of the self-lubricating coating obtained in Example 5.

[0046] Figure 7 The image shows the cross-sectional SEM morphology of the coating obtained in Comparative Example 1. Detailed Implementation

[0047] The technical solution of the present invention will be further illustrated below through specific embodiments. Those skilled in the art should understand that the embodiments described are merely illustrative of the present invention and should not be construed as limiting the invention in any way.

[0048] One embodiment of the present invention provides a self-lubricating composite coating, the self-lubricating composite coating comprising at least one composite structure.

[0049] The composite structure includes stacked AlTiX a N-layer and W 1-m Me m N layers.

[0050] The AlTiX a In layer N, X is any one or a combination of at least two of Ti, Cr, Zr, Ta, Hf, Y, Nb, Sc, Mo, V, W, Si, O, or B, and a ≤ 0.2.

[0051] The W 1-m Me m In layer N, m≤0.5, and Me is any one or at least two of Zr, Ta, Hf, Y, Nb, Sc, Mo, W or V.

[0052] The self-lubricating composite coating provided by this invention utilizes AlTiX a N-layer and W 1-m Me m The synergistic effect of the N-layer controls the diffusion process, inhibits the rapid oxidation of lubricating components, and reduces the wear rate, resulting in a coating with low friction coefficient and low wear rate. Therefore, self-lubricating composite coatings can be widely used in metal surface treatment or metal processing.

[0053] The self-lubricating composite coating provided by this invention is disposed on the surface of a substrate, wherein AlTiX a Layer N is disposed on the side closest to the substrate surface, W 1-m Me m Layer N is disposed on the side away from the substrate surface. When the self-lubricating composite coating comprises a composite structure with two or more layers, the composite structure is stacked, and the AlTiX content in each composite structure is... a The N layers are all located on the side closest to the substrate surface, W 1-m Me m All N layers are located on the side away from the substrate surface.

[0054] The W provided by this invention 1-m Me m In layer N, m ≤ 0.5; when m is 0, W 1-m Me m N layers are WN layers; when n is 0, W 1-m Me m Nth layer is W 1-m Me m layer.

[0055] In some embodiments, the AlTiX in the composite structure a The thickness of the N layer is ≤5μm, for example, it can be 1μm, 1.5μm, 2μm, 2.5μm, 3μm, 4μm or 5μm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0056] In some embodiments, W in the composite structure 1-m Me m The thickness of the N layer is ≤5μm, for example, it can be 0.1μm, 0.5μm, 1μm, 1.5μm, 2μm, 3μm, 4μm or 5μm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0057] In some embodiments, the hardness H of the self-lubricating composite coating is 18.8 GPa-38.8 GPa, for example, it can be 18.8 GPa, 20 GPa, 24 GPa, 25 GPa, 28 GPa, 30 GPa, 32 GPa, 35 GPa, 36 GPa or 38.8 GPa, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0058] In some embodiments, the elastic modulus E of the self-lubricating composite coating is 406 GPa-505 GPa, for example, it can be 406 GPa, 420 GPa, 450 GPa, 480 GPa, 500 GPa or 505 GPa, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0059] In some embodiments, the self-lubricating composite coating has a room temperature friction coefficient of 0.32-0.61 and a high temperature friction coefficient of 0.29-0.35.

[0060] In some embodiments, the room temperature wear rate of the self-lubricating composite coating is 0.52 × 10⁻⁶. -7 mm 3 / (N·m)-5.06×10 -7 mm 3 / (N·m), high-temperature wear rate is 12.3×10 -7 mm 3 / (N·m)-77.8×10 -7 mm 3 / (N·m).

[0061] In this invention, room temperature refers to 25°C and high temperature refers to 500°C.

[0062] An embodiment of the present invention provides a method for preparing a self-lubricating composite coating, the method comprising the following steps:

[0063] AlTiX was alternately sputtered by magnetron sputtering in a nitrogen-containing mixed atmosphere. a Target material and W 1-m Me m The target material is deposited on the substrate surface to obtain the self-lubricating composite coating as described in any embodiment.

[0064] The AlTiX a X in the target material is any one or a combination of at least two of Ti, Cr, Zr, Ta, Hf, Y, Nb, Sc, Mo, V, W, Si, O, or B.

[0065] The W 1-m Me m In the target material, m≤0.5, and Me is any one or a combination of at least two of Zr, Ta, Hf, Y, Nb, Sc, Mo, W or V.

[0066] The preparation method provided by this invention uses magnetron sputtering to prepare AlTiX. a N-layer and W 1-m Me m Compared to traditional arc evaporation, magnetron sputtering can deposit densely packed, smooth, and high-density thin films on the substrate surface. Moreover, the resulting films have good thickness and composition uniformity, which helps to reduce the friction coefficient and wear rate of the resulting self-lubricating composite coating.

[0067] In some embodiments, the gas in the nitrogen-containing mixed atmosphere includes nitrogen and a balance gas. The balance gas serves to maintain the absolute pressure during magnetron sputtering within the process requirements. When magnetron sputtering yields W... 1-m Me m At layer N, if the nitrogen flow rate in the nitrogen-containing mixed atmosphere is 0, then the resulting W 1-m Me m Nth layer is W 1-m Me m layer.

[0068] In some embodiments, the balancing gas includes any one or a combination of at least two of helium, neon, argon, or krypton. Typical but non-limiting combinations include a combination of helium and neon, a combination of neon and argon, a combination of argon and krypton, a combination of helium, neon, and argon, a combination of neon, argon, and krypton, or a combination of helium, neon, argon, and krypton.

[0069] In some embodiments, during magnetron sputtering, the flow rate of N2 is ≤80 sccm, for example, it can be 0 sccm, 10 sccm, 20 sccm, 40 sccm, 50 sccm, 60 sccm or 80 sccm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable, preferably ≤60 sccm.

[0070] In some embodiments, for magnetron sputtering of AlTiX a Target material and W 1-m Me m Target material, making AlTiX a Target and / or W 1- m Me m The target is fixed, and then the substrate is rotated. When the substrate rotates to the position corresponding to the target, magnetron sputtering deposition of the corresponding target is achieved.

[0071] The orbital speed affects the residence time of the matrix at the corresponding target location; the faster the orbital speed, the longer the residence time of the monolayer AlTiX. a N layers or W 1-m Me m The smaller the thickness of the Nth layer and the slower its orbital speed, the better the single-layer AlTiX... a N layers or W 1-m Me m The greater the thickness of layer N, the better.

[0072] In some embodiments, during magnetron sputtering, the substrate revolves at a speed of 0.5 rpm to 10 rpm, for example, 0.5 rpm, 1 rpm, 2 rpm, 3 rpm, 4 rpm, 5 rpm, 6 rpm, 8 rpm or 10 rpm, but is not limited to the listed values, and other unlisted values ​​within the range are also applicable.

[0073] The thickness of the coating obtained by magnetron sputtering is related to the sputtering time; the longer the time, the more revolutions the substrate makes, and the more layers of coating are obtained. By combining the substrate revolution speed and the sputtering time in this invention, the AlTiX in the composite structure can be optimized. a The thickness of layer N is ≤5μm and W 1-m Me m The thickness of the N layer is ≤5μm.

[0074] Applying a bias voltage to the substrate during magnetron sputtering attracts positive ions from the plasma to bombard the substrate under the influence of the negative bias voltage, thereby improving the deposition quality, deposition rate, and deposition uniformity.

[0075] In some embodiments, during magnetron sputtering, the bias voltage of the substrate is -50V to -500V, for example, it can be -50V, -100V, -200V, -300V, -400V or -500V, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0076] In some embodiments, the deposition temperature during magnetron sputtering is from 150°C to 450°C, for example, it can be 100°C, 150°C, 200°C, 250°C, 300°C, 350°C, 400°C or 450°C, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0077] In some embodiments, the absolute pressure during magnetron sputtering is from 0.2 Pa to 0.8 Pa, for example, it can be 0.2 Pa, 0.3 Pa, 0.4 Pa, 0.5 Pa, 0.6 Pa or 0.8 Pa, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0078] In some embodiments, magnetron sputtering of the AlTiX a Methods for using targets include DC magnetron sputtering (DCMS) or high-power pulsed magnetron sputtering (HiPIMS).

[0079] In some embodiments, magnetron sputtering of the W 1-m Me m Methods for sputtering targets include DC magnetron sputtering (DCMS), MFMS, RFMS, or HiPIMS.

[0080] In some embodiments, the AlTiX a The magnetron sputtering power of the target is 5W / cm. 2 -20W / cm 2 For example, it could be 5W / cm 2 8W / cm 2 10W / cm 2 12W / cm 2 15W / cm 2 18W / cm 2 Or 20W / cm 2 However, this does not limit the listed values; any other unlisted values ​​within the range are also applicable.

[0081] In this invention, magnetron sputtering power refers to average magnetron sputtering power.

[0082] In some embodiments, high-power pulsed magnetron sputtering is used to deposit AlTiX a The peak current density of the target material is 0.2 A / cm².2 -1A / cm 2 For example, it could be 0.2A / cm 2 0.4A / cm 2 0.5A / cm 2 0.6A / cm 2 0.8A / cm 2 or 1A / cm 2 However, this does not limit the listed values; any other unlisted values ​​within the range are also applicable.

[0083] In some embodiments, high-power pulsed magnetron sputtering of the W 1-m Me m The peak current density of the target material is 0.2 A / cm². 2 -0.8A / cm 2 For example, it could be 0.2A / cm 2 0.4A / cm 2 0.5A / cm 2 0.6A / cm 2 Or 0.8A / cm 2 However, this does not limit the listed values; any other unlisted values ​​within the range are also applicable.

[0084] In some embodiments, the substrate is pretreated before magnetron sputtering.

[0085] The pretreatment includes sequential mechanical grinding, polishing, and cleaning.

[0086] In some embodiments, the cleaning includes sequential solvent cleaning, glow discharge cleaning, and ion etching cleaning.

[0087] One embodiment of the present invention provides an application of a self-lubricating composite coating for metal surface treatment or metal processing.

[0088] The self-lubricating composite coating is any of the self-lubricating composite coatings described in any embodiment.

[0089] To clearly illustrate the technical solution of the present invention, the substrate used in the following embodiments and comparative examples is a pretreated cemented carbide substrate, wherein the pretreatment includes: firstly, mechanically grinding the substrate with sandpaper, then polishing the surface of the substrate with polishing liquid (Dongguan Yingxin Semiconductor Materials Co., Ltd., with an average diamond particle size of 2μm), and then cleaning.

[0090] The cleaning process included sequential solvent cleaning, glow discharge cleaning, and ion etching cleaning. Solvent cleaning consisted of ultrasonic cleaning with deionized water for 20 minutes, followed by ultrasonic cleaning with anhydrous ethanol for 20 minutes. Glow discharge cleaning involved 30 minutes of glow discharge cleaning in an argon atmosphere, with a working absolute pressure of 0.3 Pa, a substrate bias of -600 V, and a frequency of 30 kHz. Ion etching cleaning involved... + The substrate was cleaned with an ion source for 30 minutes at an absolute pressure of 0.3 Pa and a substrate bias voltage of -200 V.

[0091] The above description of the substrate is not intended to further limit the technical solution of the present invention.

[0092] Example 1

[0093] This embodiment provides a self-lubricating composite coating, which includes a single composite structure; the composite structure includes an AlTiN layer and a WN layer stacked together.

[0094] The method for preparing the self-lubricating composite coating provided in this embodiment includes the following steps:

[0095] (1) The flow rate of N2 was controlled to be 80 sccm, argon was used as the balance gas, and the absolute pressure of the magnetron sputtering system was controlled to be 0.6 Pa. HiPIMS magnetron sputtering was used to deposit an Al60Ti40 target material and a single layer of AlTiN with a thickness of 3 μm was deposited on the substrate surface.

[0096] The magnetron sputtering temperature was 425℃, the substrate revolution speed was 1 rpm, the substrate bias voltage was -100V, and the time was 2 hours; the magnetron sputtering power of the AlTi target was 20 W / cm². 2 The target peak current density is 1.0 A / cm². 2 The total power of HiPIMS is 8.8kW, the frequency is 1000Hz, and the pulse width is 80μs.

[0097] (2) The flow rate of N2 was controlled to 0 sccm, argon was used as the balancing gas, and the absolute pressure of the magnetron sputtering system was controlled to 0.6 Pa. A W layer with a thickness of 1.5 μm was deposited on the surface of the AlTiN monolayer coating by using HiPIMS magnetron sputtering W target.

[0098] The magnetron sputtering temperature was 425℃, the substrate revolution speed was 1 rpm, the substrate bias voltage was -100V, and the time was 1 hour; the magnetron sputtering power of the W target was 9 W / cm². 2 The target peak current density is 0.4 A / cm². 2 The total power of HiPIMS is 4kW, the frequency is 1000Hz, and the pulse width is 80μs.

[0099] The cross-sectional SEM image of the self-lubricating composite coating provided in this embodiment is as follows: Figure 2 As shown.

[0100] Example 2

[0101] This embodiment provides a self-lubricating composite coating, which includes a single composite structure; the composite structure includes an AlTiN layer and a WN layer stacked together.

[0102] The method for preparing the self-lubricating composite coating provided in this embodiment includes the following steps:

[0103] (1) The flow rate of N2 was controlled to be 80 sccm, argon was used as the balance gas, and the absolute pressure of the magnetron sputtering system was controlled to be 0.6 Pa. HiPIMS magnetron sputtering was used to deposit an Al60Ti40 target material and a single layer of AlTiN with a thickness of 2.5 μm was deposited on the substrate surface.

[0104] The parameters for sputtering AlTi targets using HiPIMS magnetron sputtering are the same as in Example 1.

[0105] (2) The flow rate of N2 was controlled to be 20 sccm, argon was used as the balancing gas, and the absolute pressure of the magnetron sputtering system was controlled to be 0.6 Pa. A WN layer with a thickness of 1.5 μm was deposited on the surface of the AlTiN monolayer coating by using HiPIMS magnetron sputtering W target.

[0106] The parameters and conditions for using the HiPIMS magnetron sputtering W target are the same as in Example 1.

[0107] The cross-sectional SEM image of the self-lubricating composite coating provided in this embodiment is as follows: Figure 3 As shown.

[0108] Example 3

[0109] This embodiment provides a self-lubricating composite coating, which includes a single composite structure; the composite structure includes an AlTiN layer and a WN layer stacked together.

[0110] The method for preparing the self-lubricating composite coating provided in this embodiment includes the following steps:

[0111] (1) The flow rate of N2 was controlled to be 80 sccm, argon was used as the balance gas, and the absolute pressure of the magnetron sputtering system was controlled to be 0.6 Pa. The Al60Ti40 target was sputtered by HiPIMS, and a single layer of AlTiN with a thickness of 2.75 μm was deposited on the substrate surface.

[0112] The parameters for sputtering AlTi targets using HiPIMS magnetron sputtering are the same as in Example 1.

[0113] (2) The flow rate of N2 was controlled to be 40 sccm, argon was used as the balancing gas, and the absolute pressure of the magnetron sputtering system was controlled to be 0.6 Pa. A WN layer with a thickness of 1.25 μm was deposited on the surface of the AlTiN monolayer coating by using HiPIMS magnetron sputtering W target.

[0114] The parameters and conditions for using the HiPIMS magnetron sputtering W target are the same as in Example 1.

[0115] The cross-sectional SEM image of the self-lubricating composite coating provided in this embodiment is as follows: Figure 4 As shown.

[0116] Example 4

[0117] This embodiment provides a self-lubricating composite coating, which includes a single composite structure; the composite structure includes an AlTiN layer and a WN layer stacked together.

[0118] The method for preparing the self-lubricating composite coating provided in this embodiment includes the following steps:

[0119] (1) The flow rate of N2 was controlled to be 80 sccm, argon was used as the balance gas, and the absolute pressure of the magnetron sputtering system was controlled to be 0.6 Pa. The Al60Ti40 target was sputtered by HiPIMS, and a single layer of AlTiN with a thickness of 3.0 μm was deposited on the substrate surface.

[0120] The parameters for sputtering AlTi targets using HiPIMS magnetron sputtering are the same as in Example 1.

[0121] (2) The flow rate of N2 was controlled to be 60 sccm, argon was used as the balancing gas, and the absolute pressure of the magnetron sputtering system was controlled to be 0.6 Pa. A WN layer with a thickness of 1.0 μm was deposited on the surface of the AlTiN monolayer coating by using HiPIMS magnetron sputtering W target.

[0122] The parameters and conditions for using the HiPIMS magnetron sputtering W target are the same as in Example 1.

[0123] The cross-sectional SEM image of the self-lubricating composite coating provided in this embodiment is as follows: Figure 5 As shown.

[0124] Example 5

[0125] This embodiment provides a self-lubricating composite coating, which includes a single composite structure; the composite structure includes an AlTiN layer and a WN layer stacked together.

[0126] The method for preparing the self-lubricating composite coating provided in this embodiment includes the following steps:

[0127] (1) The flow rate of N2 was controlled to be 80 sccm, argon was used as the balance gas, and the absolute pressure of the magnetron sputtering system was controlled to be 0.6 Pa. The Al60Ti40 target was sputtered by HiPIMS, and a single layer of AlTiN with a thickness of 3.0 μm was deposited on the substrate surface.

[0128] The parameters for sputtering AlTi targets using HiPIMS magnetron sputtering are the same as in Example 1.

[0129] (2) The flow rate of N2 was controlled to be 80 sccm, argon was used as the balance gas, and the absolute pressure of the magnetron sputtering system was controlled to be 0.6 Pa. A WN layer with a thickness of 1.1 μm was deposited on the surface of the AlTiN monolayer coating by using HiPIMS magnetron sputtering W target.

[0130] The parameters and conditions for using the HiPIMS magnetron sputtering W target are the same as in Example 1.

[0131] The cross-sectional SEM image of the self-lubricating composite coating provided in this embodiment is as follows: Figure 6 As shown.

[0132] Example 6

[0133] This embodiment provides a self-lubricating composite coating, which includes a single composite structure; the composite structure includes an AlTiN layer and a WN layer stacked together.

[0134] The method for preparing the self-lubricating composite coating provided in this embodiment includes the following steps:

[0135] (1) The flow rate of N2 was controlled to be 80 sccm, argon was used as the balancing gas, and the absolute pressure of the magnetron sputtering system was controlled to be 0.2 Pa. HiPIMS magnetron sputtering was used to deposit an Al60Ti40 target material and deposited an AlTiN single-layer coating with the same thickness as in Example 1 on the substrate surface.

[0136] The magnetron sputtering temperature was 150℃, the substrate revolution speed was 0.5 rpm, and the substrate bias voltage was -50V; the magnetron sputtering power of the AlTi target was 5W / cm². 2 The target peak current density is 0.2 A / cm². 2 The total power of HiPIMS is 8.8kW, the frequency is 1000Hz, and the pulse width is 80μs.

[0137] (2) The flow rate of N2 was controlled to 0 sccm, argon was used as the balancing gas, and the absolute pressure of the magnetron sputtering system was controlled to 0.2 Pa. HiPIMS magnetron sputtering was used to deposit a W target material on the surface of the AlTiN monolayer coating to obtain a W layer with the same thickness as in Example 1.

[0138] The magnetron sputtering temperature was 150℃, the substrate revolution speed was 0.5 rpm, and the substrate bias voltage was -50V; the magnetron sputtering power of the W target was 9 W / cm². 2 The target peak current density is 0.2 A / cm². 2 The total power of HiPIMS is 4kW, the frequency is 1000Hz, and the pulse width is 80μs.

[0139] Example 7

[0140] This embodiment provides a self-lubricating composite coating, which includes a single composite structure; the composite structure includes an AlTiN layer and a WN layer stacked together.

[0141] The method for preparing the self-lubricating composite coating provided in this embodiment includes the following steps:

[0142] (1) The flow rate of N2 was controlled to be 80 sccm, argon was used as the balance gas, and the absolute pressure of the magnetron sputtering system was controlled to be 0.8 Pa. HiPIMS magnetron sputtering was used to deposit an Al60Ti40 target material and deposited an AlTiN single-layer coating with the same thickness as in Example 1 on the substrate surface.

[0143] The magnetron sputtering temperature was 450℃, the substrate revolution speed was 10 rpm, and the substrate bias voltage was -500V; the magnetron sputtering power of the AlTi target was 20 W / cm². 2 The target peak current density is 1.0 A / cm². 2 The total power of HiPIMS is 8.8kW, the frequency is 1000Hz, and the pulse width is 80μs.

[0144] (2) The flow rate of N2 was controlled to 0 sccm, argon was used as the balancing gas, and the absolute pressure of the magnetron sputtering system was controlled to 0.2 Pa. HiPIMS magnetron sputtering was used to deposit a W target material on the surface of the AlTiN monolayer coating to obtain a W layer with the same thickness as in Example 1.

[0145] The magnetron sputtering temperature was 450℃, the substrate revolution speed was 10 rpm, and the substrate bias voltage was -500V; the magnetron sputtering power of the W target was 9 W / cm². 2 The target peak current density is 0.8 A / cm². 2 The total power of HiPIMS is 4kW, the frequency is 1000Hz, and the pulse width is 80μs.

[0146] Example 8

[0147] This embodiment provides a self-lubricating composite coating, which includes a single composite structure; the composite structure includes stacked Al layers. 0.5 Ti0.3 Cr 0.2 N-layer and W 0.5 Zr 0.5 N layers.

[0148] The method for preparing the self-lubricating composite coating provided in this embodiment includes the following steps:

[0149] (1) The flow rate of N2 was controlled at 80 sccm, argon was used as the balancing gas, and the absolute pressure of the magnetron sputtering system was controlled at 0.6 Pa. A 3 μm thick Al layer was deposited on the substrate surface using a HiPIMS magnetron sputtering Al50Ti30Cr20 target. 0.5 Ti 0.3 Cr 0.2 N single-layer coating.

[0150] The magnetron sputtering temperature was 425℃, the substrate revolution speed was 1 rpm, the substrate bias voltage was -100V, and the time was 2 hours; the magnetron sputtering power of the Al50Ti30Cr20 target was 20 W / cm². 2 The target peak current density is 1.0 A / cm². 2 The total power of HiPIMS is 8.8kW, the frequency is 1000Hz, and the pulse width is 80μs.

[0151] (2) The flow rate of N2 was controlled at 0 sccm, argon was used as the balancing gas, and the absolute pressure of the magnetron sputtering system was controlled at 0.6 Pa; HiPIMS magnetron sputtering was used to sputter W50Zr50 target material in Al 0.5 Ti 0.3 Cr 0.2 The surface deposition of the N single-layer coating yielded a W layer with a thickness of 1.5 μm. 0.5 Zr 0.5 N layers.

[0152] The magnetron sputtering temperature was 425℃, the substrate revolution speed was 1 rpm, the substrate bias voltage was -100V, and the time was 1 hour; the magnetron sputtering power of the W50Zr50 target was 9 W / cm². 2 The target peak current density is 0.4 A / cm². 2 The total power of HiPIMS is 4kW, the frequency is 1000Hz, and the pulse width is 80μs.

[0153] Example 9

[0154] This embodiment provides a self-lubricating composite coating, which includes a single composite structure; the composite structure includes stacked Al layers. 0.5 Ti 0.3 W 0.2 N-layer and W 0.5 Nb 0.5N layers.

[0155] The method for preparing the self-lubricating composite coating provided in this embodiment includes the following steps:

[0156] (1) The flow rate of N2 was controlled at 80 sccm, argon was used as the balancing gas, and the absolute pressure of the magnetron sputtering system was controlled at 0.6 Pa. A 3 μm thick Al layer was deposited on the substrate surface using a HiPIMS magnetron sputtering Al50Ti30W20 target. 0.5 Ti 0.3 W 0.2 N single-layer coating.

[0157] The magnetron sputtering temperature was 425℃, the substrate revolution speed was 1 rpm, the substrate bias voltage was -100V, and the time was 2 hours; the magnetron sputtering power of the Al50Ti30W20 target was 20 W / cm². 2 The target peak current density is 1.0 A / cm². 2 The total power of HiPIMS is 8.8kW, the frequency is 1000Hz, and the pulse width is 80μs.

[0158] (2) The flow rate of N2 was controlled at 0 sccm, argon was used as the balancing gas, and the absolute pressure of the magnetron sputtering system was controlled at 0.6 Pa; HiPIMS magnetron sputtering was used to sputter W50Nb50 target material in Al 0.5 Ti 0.3 W 0.2 The surface deposition of the N single-layer coating yielded a W layer with a thickness of 1.5 μm. 0.5 Nb 0.5 N layers.

[0159] The magnetron sputtering temperature was 425℃, the substrate revolution speed was 1 rpm, the substrate bias voltage was -100V, and the time was 1 hour; the magnetron sputtering power of the W50Nb50 target was 9 W / cm². 2 The target peak current density is 0.4 A / cm². 2 The total power of HiPIMS is 4kW, the frequency is 1000Hz, and the pulse width is 80μs.

[0160] Comparative Example 1

[0161] This comparative example provides an AlTiSiN coating, the preparation method of which includes the following steps:

[0162] The flow rate of N2 was controlled at 80 sccm, argon was used as the balance gas, and the absolute pressure of the magnetron sputtering system was controlled at 0.6 Pa; HiPIMS magnetron sputtering of Al was employed. 60 Ti 30 Si 10The target material was deposited on the substrate surface to obtain an AlTiSiN coating with a thickness of 4.0 μm.

[0163] The magnetron sputtering temperature was 425℃, the substrate revolution speed was 1 rpm, the substrate bias voltage was -100V, and the time was 2 hours; the magnetron sputtering power of the AlTi target was 20 W / cm². 2 The target peak current density is 1.0 A / cm². 2 The total power of HiPIMS is 8.8kW, the frequency is 1000Hz, and the pulse width is 80μs.

[0164] The cross-sectional SEM image of the AlTiSiN coating obtained in this comparative example is shown below. Figure 7 As shown.

[0165] Comparative Example 2

[0166] This comparative example provides a self-lubricating composite coating, which includes a single composite structure; the composite structure includes an AlTiN layer and a WTiN layer stacked together.

[0167] The method for preparing the self-lubricating composite coating provided in this comparative example includes the following steps:

[0168] (1) The flow rate of N2 was controlled to be 80 sccm, argon was used as the balance gas, and the absolute pressure of the magnetron sputtering system was controlled to be 0.6 Pa. The Al60Ti40 target was sputtered by HiPIMS, and a single layer of AlTiN with a thickness of 3.0 μm was deposited on the substrate surface.

[0169] The magnetron sputtering temperature was 425℃, the substrate revolution speed was 1 rpm, the substrate bias voltage was -100V, and the time was 2 hours; the magnetron sputtering power of the AlTi target was 20 W / cm². 2 The target peak current density is 1.0 A / cm². 2 The total power of HiPIMS is 8.8kW, the frequency is 1000Hz, and the pulse width is 80μs.

[0170] (2) The flow rate of N2 was controlled at 0 sccm, argon was used as the balance gas, and the absolute pressure of the magnetron sputtering system was controlled at 0.6 Pa; HiPIMS magnetron sputtering was used. 80 Ti 20 A WTi layer with a thickness of 2.0 μm was deposited on the surface of an AlTiN monolayer coating using a target material.

[0171] The magnetron sputtering temperature was 425℃, the substrate revolution speed was 1 rpm, the substrate bias voltage was -100V, and the time was 1 hour; W 80 Ti 20 The magnetron sputtering power of the target is 9 W / cm.2 The target peak current density is 0.4 A / cm². 2 The total power of HiPIMS is 4kW, the frequency is 1000Hz, and the pulse width is 80μs.

[0172] Performance Characterization

[0173] The hardness (H), elastic modulus (E), and oxidation resistance of the coatings obtained in the above embodiments and comparative examples were measured, and the results are shown in Table 1. The hardness (H) was determined using the nanoindentation test method, following ISO 14577-4-2017; the elastic modulus (E) was also determined using the nanoindentation test method, following ISO 14577-4-2017; the coefficient of friction was determined using a ball-and-disc friction and wear testing machine with TC4 balls (6 mm diameter), a load of 5 N, a rotation speed of 600 rpm, a maximum Hertzian stress of 1.2 GPa, and 3000 test cycles; the wear rate was determined using a ball-and-disc friction and wear testing machine, followed by observation of the wear tracks using a laser confocal microscope, measurement of the wear track depth and contour, and the wear loss volume per unit load and unit distance as the wear rate index.

[0174] Table 1

[0175]

[0176] The applicant declares that the above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A self-lubricating composite coating, characterized in that, The self-lubricating composite coating comprises at least one composite structure; The composite structure includes stacked AlTiX a N-layer and W 1-m Me m N layers; The AlTiX a In layer N, X is any one or a combination of at least two of Ti, Cr, Zr, Ta, Hf, Y, Nb, Sc, Mo, V, W, Si, O, or B, and a ≤ 0.2; The W 1-m Me m In layer N, m≤0.5, and Me is any one or at least two of Zr, Ta, Hf, Y, Nb, Sc, Mo, W or V.

2. The self-lubricating composite coating according to claim 1, characterized in that, The composite structure contains AlTiX a The thickness of the N layer is ≤5μm; And / or, in the composite structure, W 1-m Me m The thickness of the N layer is ≤5μm.

3. The self-lubricating composite coating according to claim 1 or 2, characterized in that, The hardness of the self-lubricating composite coating is 18.8 GPa-38.8 GPa; And / or, the elastic modulus of the self-lubricating composite coating is 406 GPa-505 GPa; And / or, the self-lubricating composite coating has a room temperature friction coefficient of 0.32-0.61 and a high temperature friction coefficient of 0.29-0.35; And / or, the room temperature wear rate of the self-lubricating composite coating is 0.52 × 10⁻⁶. -7 mm 3 / (N·m)-5.06×10 -7 mm 3 / (N·m), high-temperature wear rate is 12.3×10 -7 mm 3 / (N·m)-77.8×10 -7 mm 3 / (N·m).

4. A method for preparing a self-lubricating composite coating, characterized in that, The preparation method includes the following steps: AlTiX was alternately sputtered by magnetron sputtering in a nitrogen-containing mixed atmosphere. a Target material and W 1-m Me m The target material is deposited on the surface of a substrate to obtain the self-lubricating composite coating as described in any one of claims 1-3; The AlTiX a X in the target material is any one or a combination of at least two of Ti, Cr, Zr, Ta, Hf, Y, Nb, Sc, Mo, V, W, Si, O or B, and a≤0.2; The W 1-m Me m In the target material, m≤0.5, and Me is any one or a combination of at least two of Zr, Ta, Hf, Y, Nb, Sc, Mo, W or V.

5. The preparation method according to claim 4, characterized in that, The gas in the nitrogen-containing mixed atmosphere includes nitrogen and a balance gas; And / or, the balancing gas includes any one or a combination of at least two of helium, neon, argon, or krypton.

6. The preparation method according to claim 4, characterized in that, During magnetron sputtering, the flow rate of N2 is ≤80 sccm.

7. The preparation method according to any one of claims 4-6, characterized in that, During the magnetron sputtering process, the substrate revolves at a speed of 0.5 rpm to 10 rpm. And / or, during the magnetron sputtering, the substrate bias voltage is -50V to -500V; And / or, the deposition temperature during magnetron sputtering is from 150°C to 450°C; And / or, the absolute pressure during magnetron sputtering is 0.2 Pa to 0.8 Pa.

8. The preparation method according to any one of claims 4-7, characterized in that, Magnetron sputtering of AlTiX a Target methods include DC magnetron sputtering or high-power pulsed magnetron sputtering; And / or, magnetron sputtering of the W 1-m Me m Methods for sputtering targets include DC magnetron sputtering, intermediate frequency magnetron sputtering, radio frequency magnetron sputtering, or high-power pulsed magnetron sputtering.

9. The preparation method according to claim 8, characterized in that, The AlTiX a The magnetron sputtering power of the target is 5W / cm. 2 -20W / cm 2 ; And / or, high-power pulsed magnetron sputtering of the AlTiX a The peak current density of the target material is 0.2 A / cm². 2 -1A / cm 2 ; And / or, high-power pulsed magnetron sputtering of the W 1-m Me m The peak current density of the target material is 0.2 A / cm². 2 -0.8A / cm 2 .

10. A cutting tool, characterized in that, The cutting tool includes a tool body and a self-lubricating composite coating as described in any one of claims 1-3 disposed on the tool body.

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