Low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant film and preparation method thereof

Abstract

This invention discloses a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film and its preparation method. The preparation method includes: grinding and polishing the substrate; cleaning the substrate; drying the substrate; placing the substrate on the central sample stage of a magnetron sputtering instrument, mounting Ti and Cu targets on the target base, closing the sputtering chamber, and performing vacuum extraction; turning on the DC power supplies for the Ti and Cu targets respectively, and pre-sputtering the Ti and Cu targets to remove impurities adhering to their surfaces; depositing a TiCuN thin film for the first time; depositing a Cu thin film; depositing a TiCuN thin film for the second time; turning off the DC power supplies for the Ti and Cu targets, opening the vacuum valve, and removing the thin film sample. The low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film prepared by this invention has a dense, void-free surface and good, gap-free bonding between the film layers.

Description

Technical Field

[0001] This invention relates to the field of thin film preparation technology, specifically to a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film and its preparation method. Background Technology

[0002] Low infrared emissivity films are primarily coated on the surfaces of military targets to reduce their infrared emissivity, thereby achieving infrared stealth. The low infrared emissivity and high-temperature stability of the film are crucial factors affecting the infrared stealth performance of military targets. This places more stringent requirements on the selection and design of infrared stealth films. Not only must the film have low infrared emissivity, but it should also possess performance stability under high-temperature conditions, ensuring that the film maintains low infrared emissivity even at high temperatures.

[0003] Metallic thin films, especially Cu thin films, exhibit extremely low infrared emissivity. Their low cost and excellent conductivity make them a promising candidate for use as metallic emissive layers. However, Cu thin films suffer from poor high-temperature stability and are prone to oxidation and electrochemical corrosion, leading to changes in film composition and structural damage. This results in a significant increase in infrared emissivity, severely limiting their applications.

[0004] TiN possesses advantages such as high melting point, high hardness, and corrosion resistance, and exhibits lower infrared emissivity compared to other ceramic layers. Considering material compatibility, for multilayer composite films, elemental overlap in different layers is necessary to enhance the compatibility of the multilayer structure, thereby eliminating issues such as mismatched thermal expansion coefficients and interlayer element diffusion. Therefore, this invention introduces Cu into TiN to prepare a ternary TiCuN film, serving as both a protective and barrier layer for the Cu metal film. Summary of the Invention

[0005] The purpose of this invention is to provide a low-infrared-emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film and its preparation method. The Cu metal film exhibits high reflectivity to infrared radiation, resulting in a low infrared emissivity for the composite film. Ternary TiCuN thin films have attracted widespread attention due to their excellent oxidation resistance, corrosion resistance, and wear resistance, and can serve as a surface protective layer for Cu films, protecting them from chemical and mechanical damage. Furthermore, the presence of Cu in TiCuN hinders the outward diffusion of Cu from the Cu metal film, contributing to the stability of the Cu metal film. Moreover, compared to single-layer films, the multi-layer design further reduces the infrared emissivity of the composite film.

[0006] The present invention is achieved using the following technical solution:

[0007] A method for preparing a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film includes the following steps:

[0008] Step 1: First, use sandpaper to mechanically sand the substrate, then polish it until the surface is free of obvious scratches and has a mirror finish.

[0009] Step 2: Immerse the matrix obtained in Step 1 in an ethanol solution for ultrasonic excitation, and then immerse it in deionized water for ultrasonic cleaning.

[0010] Step 3: Wipe the surface of the substrate obtained in Step 2 clean and then dry it.

[0011] Step 4: Place the substrate obtained in step 3 on the central sample stage of the magnetron sputtering instrument, install Ti and Cu targets on the target base, close the sputtering chamber, and after confirming that all steps are correct, perform vacuum extraction.

[0012] Step 5, when the vacuum in step 4 reaches the background vacuum of 7.0 × 10⁻⁶ -4 After Pa, open the argon valve to introduce argon gas, and then turn on the DC power supply for Ti and Cu targets respectively to pre-sputter the Ti and Cu targets to remove impurities attached to the surface of the Ti and Cu targets.

[0013] Step 6: After the pre-sputtering in Step 5 is completed, set the sputtering parameters for the TiCuN thin film, open the nitrogen valve, turn on the DC power supply for the Ti and Cu targets, and perform reactive magnetron co-sputtering to deposit the TiCuN thin film.

[0014] Step 7: After the sputtering in Step 6 is completed, close the nitrogen and argon valves, perform vacuum extraction, and after the nitrogen and argon in the sputtering chamber are completely removed, set the Cu thin film sputtering parameters, open the argon valve, turn on the Cu target DC power supply, and deposit the Cu thin film.

[0015] Step 8: After the sputtering in step 7 is completed, set the same sputtering parameters as in step 6 for the TiCuN thin film, open the nitrogen valve, turn on the DC power supply for the Ti and Cu targets, and perform reactive magnetron co-sputtering to deposit the TiCuN thin film.

[0016] Step 9: After the sputtering in step 8 is completed, turn off the DC power supply to the Ti and Cu targets, open the vacuum valve, and remove the thin film sample.

[0017] A further improvement of the present invention is that, in step 1, the substrate material is selected from glass, silicon wafer, high-speed steel or stainless steel, with a size of 20.0×20.0×1.0mm. The high-speed steel or stainless steel is polished with sandpaper from coarse to fine, and then polished.

[0018] A further improvement of the present invention is that, in step 2, the ultrasonic excitation time of the ethanol solution is 5-10 min, and the ultrasonic cleaning time of the deionized water is 10-20 min.

[0019] A further improvement of the present invention is that the drying temperature of the substrate in step 3 is 50-80°C and the drying time is 60-100 min.

[0020] A further improvement of this invention is that, in step 4, the purity of the Ti target is 99.999%, and the purity of the Cu target is 99.999%. When the Ti and Cu targets are mounted on the target base, they are placed at a 45° angle relative to each other. The distance between the substrate and the sputtering target is adjusted to 40-60 mm, and no bias voltage is applied to the target. When evacuating the vacuum, the mechanical pump and the pre-evacuation valve are opened first to perform low vacuum evacuation. When the gas pressure in the sputtering chamber is lower than 0.5 Pa, the pre-evacuation valve is closed, and the fore-stage valve, molecular pump, and gate valve are opened in sequence to perform high vacuum evacuation.

[0021] A further improvement of the present invention is that, in step 5, before turning on the DC power supply to the Ti and Cu targets, the substrate baffle is opened to protect the substrate material from contamination by pre-sputtered atoms. The pre-sputtering argon flow rate is 20-50 sccm, the sputtering pressure is 0.1-0.5 Pa, the sputtering power is 50-200 W, and the sputtering time is 20-60 min.

[0022] A further improvement of the present invention is that, after the pre-sputtering in step 6, the substrate baffle is closed, and the sputtering parameters of the TiCuN thin film are set as follows: nitrogen flow rate is 1-8 sccm, Ti target sputtering power is 80-200 W, Cu target sputtering power is 50-100 W, co-sputtering deposition time is 10-60 min, and substrate temperature is room temperature.

[0023] A further improvement of this invention is that the vacuum background in step 7 is 7.0 × 10⁻⁶. -4 The sputtering power of the Pa and Cu targets was 50–80 W, the deposition time was 10–40 min, and the substrate temperature was room temperature.

[0024] A further improvement of the present invention is that, in step 9, the number of layers is 3, the innermost and outermost layers are both TiCuN films, the middle layer is a Cu film, and the total film thickness is 0.5 to 1 μm.

[0025] A low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film is prepared by the aforementioned method for preparing a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film.

[0026] The present invention has at least the following beneficial technical effects:

[0027] 1. This invention relates to a low-infrared-emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film and its preparation method. The method employs magnetron sputtering to prepare a three-layer, nano-sized low-infrared-emissivity TiCuN / Cu / TiCuN corrosion-resistant composite thin film with a thickness of less than 1 μm. Using a metallic Cu film as the inner emitting layer reduces the infrared emissivity of the composite film. Using a TiCuN film as the surface layer improves the composite film's oxidation resistance, wear resistance, and corrosion resistance, thereby extending the lifespan of the TiCuN / Cu / TiCuN thin film.

[0028] 2. This invention relates to a low-infrared-emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film and its preparation method. By introducing Cu into the low-infrared-emissivity TiN thin film, a ternary TiCuN thin film is prepared. This not only maintains its low infrared emissivity but also acts as a barrier layer for the metallic Cu thin film, eliminating problems such as mismatch of thermal expansion coefficients and interlayer element diffusion in the TiCuN / Cu / TiCuN film, thereby improving the stability of the TiCuN / Cu / TiCuN thin film.

[0029] 3. The low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film prepared by this invention has a dense, void-free surface and good, gap-free bonding between film layers. Compared with single-layer TiCuN and Cu metal films, its infrared emissivity and corrosion resistance are improved to varying degrees. Attached Figure Description

[0030] Figure 1 This is the XRD pattern of the thin film prepared according to the present invention;

[0031] Figure 2 Here is a surface SEM image of the thin film prepared according to the present invention;

[0032] Figure 3 This is an infrared emissivity diagram of the thin film prepared according to the present invention. Detailed Implementation

[0033] Exemplary embodiments of the present disclosure will now be described in more detail with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be implemented in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided to enable a more thorough understanding of the present disclosure and to fully convey the scope of the disclosure to those skilled in the art. It should be noted that, unless otherwise specified, the embodiments and features described herein can be combined with each other. The present invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0034] This invention relates to a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film and its preparation method, which are specifically implemented according to the following steps:

[0035] Step 1: Grind the high-speed steel or stainless steel substrate with dimensions of 20.0×20.0×1.0mm using sandpaper ranging from coarse to fine, and then polish it.

[0036] Step 2: Immerse the matrix obtained in Step 1 in an ethanol solution for ultrasonic excitation for 5-10 minutes, and then immerse it in deionized water for ultrasonic cleaning for 10-20 minutes.

[0037] Step 3: Wipe the surface of the substrate obtained in Step 2 clean with microscope lens paper, and dry it in a forced-air drying oven at 50-80℃ for 60-100 minutes.

[0038] Step 4: Place the substrate obtained in Step 3 on the sample stage of the magnetron sputtering instrument. Install Ti and Cu targets with a purity of 99.999% on the target base respectively. Ti and Cu targets are placed at a 45° angle relative to each other. Adjust the distance between the substrate and the sputtering target to 40-60 mm. Do not apply bias voltage to the target. Close the sputtering chamber. After confirming that all steps are correct, first open the mechanical pump and pre-evacuation valve to perform low vacuum evacuation. When the gas pressure in the sputtering chamber is lower than 0.5 Pa, close the pre-evacuation valve and then open the fore-stage valve, molecular pump and gate valve in sequence to perform high vacuum evacuation.

[0039] Step 5, when the vacuum in step 4 reaches the background vacuum of 7.0 × 10⁻⁶ -4 After Pa, set the argon flow rate to 20-50 sccm, the sputtering pressure to 0.1-0.5 Pa, and the sputtering power of Ti and Cu targets to 50-200 W. Open the substrate baffle, open the argon valve to introduce argon, turn on the DC power supply of Ti and Cu targets, and pre-sputter the Ti and Cu targets for 20-60 min to remove impurities attached to the surface of Ti and Cu targets.

[0040] Step 6: After the pre-sputtering in Step 5 is completed, set the nitrogen flow rate to 1-8 sccm, the Ti target sputtering power to 80-200 W, the Cu target sputtering power to 50-100 W, the co-sputtering deposition time to 10-60 min, the substrate temperature to room temperature, close the substrate baffle, open the nitrogen valve to introduce nitrogen, turn on the DC power supply for the Ti target and Cu target, and perform reactive magnetron co-sputtering to deposit a TiCuN thin film.

[0041] Step 7: After the sputtering in Step 6 is completed, close the nitrogen valve and perform vacuum evacuation. When the vacuum background reaches 7.0 × 10⁻⁶... -4 At Pa, the Cu target sputtering power is set to 50-80W, the deposition time to 10-40min, the substrate temperature to room temperature, the Cu target DC power supply is turned on, and Cu thin film is deposited by magnetron DC sputtering.

[0042] Step 8: After the sputtering in step 7 is completed, set the same sputtering parameters as in step 6 for the TiCuN thin film, open the nitrogen valve, turn on the DC power supply for the Ti and Cu targets, and perform reactive magnetron co-sputtering to deposit the TiCuN thin film.

[0043] Step 9: After the sputtering in step 8 is completed, turn off the DC power supply to the Ti and Cu targets, open the vacuum valve, and remove the thin film sample.

[0044] Example 1

[0045] Step 1: Grind the high-speed steel or stainless steel substrate with dimensions of 20.0×20.0×1.0mm using sandpaper ranging from coarse to fine, and then polish it.

[0046] Step 2: Immerse the matrix obtained in Step 1 in an ethanol solution for ultrasonic excitation for 8 minutes, and then immerse it in deionized water for ultrasonic cleaning for 15 minutes.

[0047] Step 3: Wipe the surface of the substrate obtained in Step 2 clean with microscope lens paper, and dry it in a forced-air drying oven at 80°C for 60 minutes.

[0048] Step 4: Place the substrate obtained in Step 3 on the sample stage of the magnetron sputtering instrument. Install Ti and Cu targets with a purity of 99.999% on the target base respectively. Ti and Cu targets are tilted at a 45° angle relative to each other. Adjust the distance between the substrate and the sputtering target to 55 mm. Do not apply bias voltage to the target. Close the sputtering chamber. After confirming that all steps are correct, first open the mechanical pump and pre-evacuation valve to perform low vacuum evacuation. When the gas pressure in the sputtering chamber is lower than 0.5 Pa, close the pre-evacuation valve and then open the fore-stage valve, molecular pump and gate valve in sequence to perform high vacuum evacuation.

[0049] Step 5, when the vacuum in step 4 reaches the background vacuum of 7.0 × 10⁻⁶ -4 After Pa, set the argon flow rate to 40 sccm, the sputtering pressure to 0.3 Pa, and the sputtering power of Ti and Cu targets to 80 W. Open the substrate baffle, open the argon valve to introduce argon, turn on the DC power supply of Ti and Cu targets, and pre-sputter the Ti and Cu targets for 30 min to remove impurities attached to the surface of Ti and Cu targets.

[0050] Step 6: After the pre-sputtering in Step 5 is completed, set the nitrogen flow rate to 2 sccm, the Ti target sputtering power to 100W, the Cu target sputtering power to 60W, the co-sputtering deposition time to 20 min, the substrate temperature to room temperature, close the substrate baffle, open the nitrogen valve to introduce nitrogen, turn on the DC power supply for the Ti target and Cu target, and perform reactive magnetron co-sputtering to deposit a TiCuN thin film.

[0051] Step 7: After the sputtering in Step 6 is completed, close the nitrogen valve and perform vacuum evacuation. When the vacuum background reaches 7.0 × 10⁻⁶... -4 At Pa, the Cu target sputtering power was set to 60W, the deposition time to 15min, the substrate temperature to room temperature, the Cu target DC power supply was turned on, and Cu thin film was deposited by magnetron DC sputtering.

[0052] Step 8: After the sputtering in step 7 is completed, set the same sputtering parameters as in step 6 for the TiCuN thin film, open the nitrogen valve, turn on the DC power supply for the Ti and Cu targets, and perform reactive magnetron co-sputtering to deposit the TiCuN thin film.

[0053] Step 9: After the sputtering in step 8 is completed, turn off the DC power supply to the Ti and Cu targets, open the vacuum valve, and remove the thin film sample.

[0054] Example 2

[0055] Step 1: Grind the high-speed steel or stainless steel substrate with dimensions of 20.0×20.0×1.0mm using sandpaper ranging from coarse to fine, and then polish it.

[0056] Step 2: Immerse the matrix obtained in Step 1 in an ethanol solution for ultrasonic excitation for 8 minutes, and then immerse it in deionized water for ultrasonic cleaning for 15 minutes.

[0057] Step 3: Wipe the surface of the substrate obtained in Step 2 clean with microscope lens paper, and dry it in a forced-air drying oven at 80°C for 60 minutes.

[0058] Step 4: Place the substrate obtained in Step 3 on the sample stage of the magnetron sputtering instrument. Install Ti and Cu targets with a purity of 99.999% on the target base respectively. Ti and Cu targets are tilted at a 45° angle relative to each other. Adjust the distance between the substrate and the sputtering target to 55 mm. Do not apply bias voltage to the target. Close the sputtering chamber. After confirming that all steps are correct, first open the mechanical pump and pre-evacuation valve to perform low vacuum evacuation. When the gas pressure in the sputtering chamber is lower than 0.5 Pa, close the pre-evacuation valve and then open the fore-stage valve, molecular pump and gate valve in sequence to perform high vacuum evacuation.

[0059] Step 5: After the vacuum in Step 4 reaches the background vacuum of 7.0×10-4Pa, set the argon flow rate to 40sccm, the sputtering pressure to 0.3Pa, and the sputtering power of Ti and Cu targets to 80W. Open the substrate baffle, open the argon valve to introduce argon, turn on the DC power supply of Ti and Cu targets, and pre-sputter the Ti and Cu targets for 30min to remove impurities attached to the surface of Ti and Cu targets.

[0060] Step 6: After the pre-sputtering in Step 5 is completed, set the nitrogen flow rate to 2 sccm, the Ti target sputtering power to 100W, the Cu target sputtering power to 60W, the co-sputtering deposition time to 20 min, the substrate temperature to room temperature, close the substrate baffle, open the nitrogen valve to introduce nitrogen, turn on the DC power supply for the Ti target and Cu target, and perform reactive magnetron co-sputtering to deposit a TiCuN thin film.

[0061] Step 7: After the sputtering in Step 6 is completed, close the nitrogen valve and perform vacuum extraction. When the vacuum background reaches 7.0×10-4 Pa, set the Cu target sputtering power to 60W, the deposition time to 25min, the substrate temperature to room temperature, turn on the Cu target DC power supply, and deposit the Cu thin film by magnetron DC sputtering.

[0062] Step 8: After the sputtering in step 7 is completed, set the same sputtering parameters as in step 6 for the TiCuN thin film, open the nitrogen valve, turn on the DC power supply for the Ti and Cu targets, and perform reactive magnetron co-sputtering to deposit the TiCuN thin film.

[0063] Step 9: After the sputtering in step 8 is completed, turn off the DC power supply to the Ti and Cu targets, open the vacuum valve, and remove the thin film sample.

[0064] Example 3

[0065] Step 1: Grind the high-speed steel or stainless steel substrate with dimensions of 20.0×20.0×1.0mm using sandpaper ranging from coarse to fine, and then polish it.

[0066] Step 2: Immerse the matrix obtained in Step 1 in an ethanol solution for ultrasonic excitation for 8 minutes, and then immerse it in deionized water for ultrasonic cleaning for 15 minutes.

[0067] Step 3: Wipe the surface of the substrate obtained in Step 2 clean with microscope lens paper, and dry it in a forced-air drying oven at 80°C for 60 minutes.

[0068] Step 4: Place the substrate obtained in Step 3 on the sample stage of the magnetron sputtering instrument. Install Ti and Cu targets with a purity of 99.999% on the target base respectively. Ti and Cu targets are tilted at a 45° angle relative to each other. Adjust the distance between the substrate and the sputtering target to 55 mm. Do not apply bias voltage to the target. Close the sputtering chamber. After confirming that all steps are correct, first open the mechanical pump and pre-evacuation valve to perform low vacuum evacuation. When the gas pressure in the sputtering chamber is lower than 0.5 Pa, close the pre-evacuation valve and then open the fore-stage valve, molecular pump and gate valve in sequence to perform high vacuum evacuation.

[0069] Step 5, when the vacuum in step 4 reaches the background vacuum of 7.0 × 10⁻⁶ -4After Pa, set the argon flow rate to 40 sccm, the sputtering pressure to 0.3 Pa, and the sputtering power of Ti and Cu targets to 80 W. Open the substrate baffle, open the argon valve to introduce argon, turn on the DC power supply of Ti and Cu targets, and pre-sputter the Ti and Cu targets for 30 min to remove impurities attached to the surface of Ti and Cu targets.

[0070] Step 6: After the pre-sputtering in Step 5 is completed, set the nitrogen flow rate to 2 sccm, the Ti target sputtering power to 100W, the Cu target sputtering power to 60W, the co-sputtering deposition time to 20 min, the substrate temperature to room temperature, close the substrate baffle, open the nitrogen valve to introduce nitrogen, turn on the DC power supply for the Ti target and Cu target, and perform reactive magnetron co-sputtering to deposit a TiCuN thin film.

[0071] Step 7: After the sputtering in Step 6 is completed, close the nitrogen valve and perform vacuum evacuation. When the vacuum background reaches 7.0 × 10⁻⁶... -4 At Pa, the Cu target sputtering power was set to 60W, the deposition time to 40min, the substrate temperature to room temperature, the Cu target DC power supply was turned on, and Cu thin film was deposited by magnetron DC sputtering.

[0072] Step 8: After the sputtering in step 7 is completed, set the same sputtering parameters as in step 6 for the TiCuN thin film, open the nitrogen valve, turn on the DC power supply for the Ti and Cu targets, and perform reactive magnetron co-sputtering to deposit the TiCuN thin film.

[0073] Step 9: After the sputtering in step 8 is completed, turn off the DC power supply to the Ti and Cu targets, open the vacuum valve, and remove the thin film sample.

[0074] Example 4

[0075] Step 1: Grind the high-speed steel or stainless steel substrate with dimensions of 20.0×20.0×1.0mm using sandpaper ranging from coarse to fine, and then polish it.

[0076] Step 2: Immerse the matrix obtained in Step 1 in an ethanol solution for ultrasonic excitation for 8 minutes, and then immerse it in deionized water for ultrasonic cleaning for 15 minutes.

[0077] Step 3: Wipe the surface of the substrate obtained in Step 2 clean with microscope lens paper, and dry it in a forced-air drying oven at 80°C for 60 minutes.

[0078] Step 4: Place the substrate obtained in Step 3 on the sample stage of the magnetron sputtering instrument. Install Ti and Cu targets with a purity of 99.999% on the target base respectively. Ti and Cu targets are tilted at a 45° angle relative to each other. Adjust the distance between the substrate and the sputtering target to 55 mm. Do not apply bias voltage to the target. Close the sputtering chamber. After confirming that all steps are correct, first open the mechanical pump and pre-evacuation valve to perform low vacuum evacuation. When the gas pressure in the sputtering chamber is lower than 0.5 Pa, close the pre-evacuation valve and then open the fore-stage valve, molecular pump and gate valve in sequence to perform high vacuum evacuation.

[0079] Step 5, when the vacuum in step 4 reaches the background vacuum of 7.0 × 10⁻⁶ -4 After Pa, set the argon flow rate to 40 sccm, the sputtering pressure to 0.3 Pa, and the sputtering power of Ti and Cu targets to 80 W. Open the substrate baffle, open the argon valve to introduce argon, turn on the DC power supply of Ti and Cu targets, and pre-sputter the Ti and Cu targets for 30 min to remove impurities attached to the surface of Ti and Cu targets.

[0080] Step 6: After the pre-sputtering in Step 5 is completed, set the nitrogen flow rate to 2 sccm, the Ti target sputtering power to 100W, the Cu target sputtering power to 100W, the co-sputtering deposition time to 20 min, the substrate temperature to room temperature, close the substrate baffle, open the nitrogen valve to introduce nitrogen, turn on the DC power supply for the Ti target and Cu target, and perform reactive magnetron co-sputtering to deposit a TiCuN thin film.

[0081] Step 7: After the sputtering in Step 6 is completed, close the nitrogen valve and perform vacuum evacuation. When the vacuum background reaches 7.0 × 10⁻⁶... -4 At Pa, the Cu target sputtering power was set to 100W, the deposition time to 30min, the substrate temperature to room temperature, the Cu target DC power supply was turned on, and Cu thin film was deposited by magnetron DC sputtering.

[0082] Step 8: After the sputtering in step 7 is completed, set the same sputtering parameters as in step 6 for the TiCuN thin film, open the nitrogen valve, turn on the DC power supply for the Ti and Cu targets, and perform reactive magnetron co-sputtering to deposit the TiCuN thin film.

[0083] Step 9: After the sputtering in step 8 is completed, turn off the DC power supply to the Ti and Cu targets, open the vacuum valve, and remove the thin film sample.

[0084] This invention provides a low-infrared-emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film and its preparation method. The method utilizes magnetron sputtering technology to prepare a three-layer, less than 1 μm thick, nano-scale low-infrared-emissivity TiCuN / Cu / TiCuN corrosion-resistant composite thin film. By using a TiCuN film as the surface and barrier layer, and a Cu film as the inner emitting layer, the film structure is optimized, which not only reduces the infrared emissivity of the film but also improves its chemical, mechanical, and thermal stability.

[0085] like Figure 1 The image shows the XRD pattern of the TiCuN / Cu / TiCuN thin film prepared in this invention. Diffraction peaks of TiCuN and Cu phases can be observed, and no other impurity peaks were detected, indicating that the prepared thin film is composed of two phases, TiCuN and Cu.

[0086] like Figure 2 As shown, the surface SEM image of the TiCuN / Cu / TiCuN thin film prepared by this invention shows that the film surface is flat, the particle size is uniform, and it is dense and pore-free, which can greatly improve the corrosion resistance of the film.

[0087] like Figure 3 As shown in the infrared emissivity diagram of the sample in Case 3 prepared by the present invention, through optimization of the film structure and composition, the infrared emissivity of both is between 0.1 and 0.2 compared with Cu film. The infrared emissivity value of TiCuN / Cu / TiCuN film prepared by the present invention is close to that of Cu film, indicating that the method provided by the present invention can not only maintain the low infrared emissivity of Cu film, but also effectively solve the problems of easy oxidation and corrosion of Cu film.

[0088] Although the present invention has been described in detail above with general descriptions and specific embodiments, modifications or improvements can be made to it, which will be obvious to those skilled in the art. Therefore, all such modifications or improvements made without departing from the spirit of the present invention fall within the scope of protection claimed by the present invention.

Claims

1. A method for preparing a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film, characterized in that, Includes the following steps: Step 1: First, use sandpaper to mechanically sand the substrate, then polish it until the surface is free of obvious scratches and has a mirror finish. Step 2: Immerse the matrix obtained in Step 1 in an ethanol solution for ultrasonic excitation, and then immerse it in deionized water for ultrasonic cleaning. Step 3: Wipe the surface of the substrate obtained in Step 2 clean and then dry it. Step 4: Place the substrate obtained in step 3 on the central sample stage of the magnetron sputtering instrument, install Ti and Cu targets on the target base, close the sputtering chamber, and after confirming that all steps are correct, perform vacuum extraction. Step 5, when the vacuum in step 4 reaches the background vacuum of 7.0 × 10⁻⁶ -4 After Pa, open the argon valve to introduce argon gas, and then turn on the DC power supply for Ti and Cu targets respectively to pre-sputter the Ti and Cu targets to remove impurities attached to the surface of the Ti and Cu targets. Step 6: After the pre-sputtering in Step 5 is completed, set the sputtering parameters for the TiCuN thin film, open the nitrogen valve, turn on the DC power supply for the Ti and Cu targets, and perform reactive magnetron co-sputtering to deposit the TiCuN thin film. Step 7: After the sputtering in Step 6 is completed, close the nitrogen and argon valves, perform vacuum extraction, and after the nitrogen and argon in the sputtering chamber are completely removed, set the Cu thin film sputtering parameters, open the argon valve, turn on the Cu target DC power supply, and deposit the Cu thin film. Step 8: After the sputtering in step 7 is completed, set the same sputtering parameters as in step 6 for the TiCuN thin film, open the nitrogen valve, turn on the DC power supply for the Ti and Cu targets, and perform reactive magnetron co-sputtering to deposit the TiCuN thin film. Step 9: After the sputtering in step 8 is completed, turn off the DC power supply to the Ti and Cu targets, open the vacuum valve, and remove the thin film sample.

2. The method for preparing a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film according to claim 1, characterized in that, In step 1, the substrate material is selected from glass, silicon wafer, high-speed steel or stainless steel, with a size of 20.0×20.0×1.0mm. The high-speed steel or stainless steel is polished with sandpaper from coarse to fine, and then polished.

3. The method for preparing a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film according to claim 1, characterized in that, In step 2, the ultrasonic excitation time for the ethanol solution is 5-10 min, and the ultrasonic cleaning time for the deionized water is 10-20 min.

4. The method for preparing a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film according to claim 1, characterized in that, In step 3, the drying temperature of the substrate is 50~80℃ and the drying time is 60~100 min.

5. The method for preparing a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film according to claim 1, characterized in that, In step 4, the purity of the Ti target is 99.999%, and the purity of the Cu target is 99.999%. When mounting the Ti and Cu targets on the target base, the Ti and Cu targets are placed at a 45° angle relative to each other. The distance between the substrate and the sputtering target is adjusted to 40~60mm, and no bias voltage is applied to the target. When evacuating the vacuum, the mechanical pump and the pre-evacuation valve are opened first to perform low vacuum evacuation. When the gas pressure in the sputtering chamber is lower than 0.5Pa, the pre-evacuation valve is closed, and the fore-stage valve, molecular pump and gate valve are opened in sequence to perform high vacuum evacuation.

6. The method for preparing a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film according to claim 1, characterized in that, Before turning on the DC power supply for the Ti and Cu targets in step 5, open the substrate baffle to protect the substrate material from contamination by pre-sputtered atoms. The pre-sputtering argon flow rate is 20~50 sccm, the sputtering pressure is 0.1~0.5 Pa, the sputtering power is 50~200 W, and the sputtering time is 20~60 min.

7. The method for preparing a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film according to claim 1, characterized in that, After pre-sputtering in step 6, the substrate baffle is closed, and the sputtering parameters of the TiCuN thin film are set as follows: nitrogen flow rate is 1~8 sccm, Ti target sputtering power is 80~200W, Cu target sputtering power is 50~100W, co-sputtering deposition time is 10~60min, and substrate temperature is room temperature.

8. The method for preparing a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film according to claim 1, characterized in that, The vacuum background in step 7 is 7.0 × 10⁻⁶. -4 The sputtering power of the Pa and Cu target is 50~80W, the deposition time is 10~40min, and the substrate temperature is room temperature.

9. The method for preparing a low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film according to claim 1, characterized in that, Step 9: There are 3 layers. The innermost and outermost layers are TiCuN films, and the middle layer is a Cu film. The total film thickness is 0.5~1μm.

10. A low infrared emissivity TiCuN / Cu / TiCuN corrosion-resistant thin film, prepared by the preparation method of any one of claims 1 to 9.

Images