Method for preparing TiAlSiN nano composite film by adopting high-power pulse magnetron sputtering
Through high-power pulsed magnetron sputtering and arc-enhanced glow discharge technology, combined with process parameter regulation, TiAlSiN nanocomposite film was prepared, which solved the problems of insufficient film uniformity, binding force and flatness in the prior art, and achieved high hardness and wear resistance.
Patent Information
- Application Number
- CN202510400180.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-01
- Publication Date
- 2025-06-27
AI Technical Summary
In the prior art, when preparing TiAlSiN nanocomposite films, there are problems such as poor uniformity of the film layer, insufficient binding force, decreased flatness and low deposition rate.
High-power pulse magnetron sputtering technology combined with arc-enhanced glow discharge technology, Ti-Al-Si-N nanocomposite film is prepared by etching, cleaning of the matrix materials and controlling key process parameters during coating.
The preparation of high hardness, good toughness, wear resistance and high-quality coatings has been achieved, the film-based bonding performance and the flatness of the film have been improved, and the defects in traditional technology have been solved.
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Abstract
Description
Technical Field
[0001] The present invention relates to the field of preparation of metal thin film materials, and particularly to a method for preparing TiAlSiN nanocomposite thin films by high-power pulsed magnetron sputtering. Background Art
[0002] With the development of advanced machining technologies such as high-speed cutting and green dry cutting, and the wide application of difficult-to-machine materials, the cutting environment of tools has become increasingly harsh, and tool coating materials have been continuously updated. At present, the tool coating technology has become one of the key factors to improve the technical level of the manufacturing industry and reduce costs and increase efficiency for enterprises. As a new type of nanocomposite coating, titanium aluminum silicon nitride (TiAlSiN) has advantages such as high hardness, low friction coefficient, and excellent high-temperature oxidation resistance. It can improve the cutting efficiency, service life, and workpiece surface integrity of tools, broaden the application range of tools in the field of high-speed machining, and has become a research hotspot for tool coatings.
[0003] At present, the preparation of TiAlSiN coatings in production mainly uses traditional direct current magnetron sputtering and multi-arc ion plating technologies. However, direct current magnetron sputtering uses a direct current power supply, with low metal ionization rate, insufficient bonding force, poor film layer uniformity, and possible shadow effects; the characteristics of arc discharge in multi-arc ion plating are prone to form large particle defects on the coating surface, resulting in a serious decline in the flatness and film-substrate bonding force of the thin film. At the same time, the phenomenon of "target poisoning" is likely to occur during the coating process. High-power pulsed magnetron sputtering technology (HiPIMS) is a new physical vapor deposition technology that uses a pulsed power supply on the basis of traditional magnetron sputtering technology, effectively improving the deficiencies of traditional magnetron sputtering technology. Its characteristics are: high pulsed peak power (2-3 orders of magnitude higher than traditional ones), low pulse duty cycle, low average power, extremely high ionization rate, which is more conducive to controlling the energy and direction of deposited particles, obtaining dense high-quality coatings, reducing residual stress, obtaining excellent film-substrate bonding performance, and making the microstructure of the coating controllable, thereby optimizing to obtain the required performance, and having broad application prospects in the coating preparation of advanced cutting tools, precision forming dies, key mechanical components, etc.
[0004] Arc-enhanced glow discharge (AEGD) ion cleaning and etching technology is a method of surface treatment by generating a high-density electron flow through arc discharge. Under the traction of the anode rod, the electron flow ionizes argon gas in the chamber into high-density argon ions, and these ions bombard the sample surface under the action of the negative bias voltage of the substrate, thereby efficiently cleaning the residual impurities, oxides, and other substances that may affect the film adhesion on the surface. Compared with traditional metal ion etching, AEGD technology effectively avoids damage to the sample surface, does not leave large particle metal defects to affect the subsequent coating quality, significantly reduces the impurities on the substrate surface, and also has a pre-ionization effect on the reaction gas used in the subsequent coating.
[0005] The combined etching and pre-ionization functions of the arc-enhanced glow discharge technology are used in the high-power pulsed magnetron sputtering technology with a high sputtering ionization rate, which not only ensures excellent adhesion of the coating, but also is easy to control the deposition process, makes up for the deficiency of the low deposition rate of the HiPIMS process, and improves the coating uniformity of workpieces with complex structures, which is beneficial to the preparation of high-quality and high-performance hard coatings. Summary of the Invention
[0006] The purpose of the present invention is to overcome the above-mentioned shortcomings and deficiencies of the prior art, and provide a method for preparing TiAlSiN nanocomposite thin films by high-power pulsed magnetron sputtering. The present invention optimizes the film-substrate bonding strength and comprehensive performance of the Ti-Al-Si-N nanocomposite thin film deposited by high-power pulsed magnetron sputtering. By etching and cleaning the substrate material and regulating key process parameters such as the substrate negative bias and target power during the coating process, the present invention realizes the controllable preparation of Ti-Al-Si-N nanocomposite thin films with good bonding to the substrate, high hardness, good toughness, and high wear resistance.
[0007] The present invention is realized through the following technical solutions:
[0008] A method for preparing TiAlSiN nanocomposite thin films by high-power pulsed magnetron sputtering, comprising the following steps:
[0009] S1, surface pretreatment of the workpiece substrate and loading into the furnace: The workpiece substrate to be coated is subjected to surface treatment, and then the surface-treated workpiece substrate is placed in the furnace cavity of the PVD deposition equipment.
[0010] S2, evacuation and heating of the furnace cavity: Seal the chamber of the vacuum furnace cavity, start the evacuation, evacuate to a base vacuum of 4.0×10 -5 mbar, then turn on the infrared heating tube for heating, and pre-treat the workpiece substrate plasma etching by heating and evacuating multiple times.
[0011] S3, plasma etching of the workpiece substrate surface: After completing the pretreatment operation in step S2, turn on the arc-enhanced glow discharge to perform plasma etching and cleaning on the workpiece substrate, continuously introduce high-purity Ar gas into the chamber to keep the chamber pressure at 1×10 -2 mbar, and apply a pulsed bias voltage to the workpiece substrate.
[0012] S4, sputtering coating on the workpiece substrate surface: Introduce a fixed ratio of high-purity Ar gas and high-purity N2 into the vacuum chamber, keep the temperature of the infrared heating tube in the chamber constant, apply a DC bias voltage to the workpiece substrate, use high-power pulsed magnetron sputtering, apply a pulsed bias voltage to the target, and perform a coating treatment for 180 min to deposit a 1-2 μm thick TiAlSiN nanocomposite hard film.
[0013] S5, Chamber Cooling and Sampling: After the sputtering coating is completed, switch the circulating cold and hot water in the furnace chamber to cold water at 16°C - 18°C to cool the chamber. When the temperature in the vacuum chamber drops below 70°C, the workpiece substrate can be taken out to complete the TiAlSiN thin film on the surface of the workpiece substrate.
[0014] In the above step S1, the surface treatment of the workpiece substrate means that the surface of the workpiece substrate is mirror-like smooth, and the surface roughness Ra value is lower than 0.4μm.
[0015] In the above step S2, the pre-treatment of the plasma etching of the workpiece substrate refers to removing the moisture, trace gases and volatile impurities inside the workpiece substrate, the bracket carrying the workpiece substrate, and the chamber.
[0016] In the above step S2, the infrared heating tubes cover the entire rear wall of the chamber and heat the inside of the chamber by thermal radiation. The actual temperature inside the chamber is measured by the thermocouple on the left front side of the chamber and is set at three measurement points, upper, middle and lower, in the chamber.
[0017] In the above step S2, before pumping to the base vacuum of 4.0×10 -5 mbar, it is necessary to first use a mechanical pump to pump to a low vacuum of 2.0×10 -5 mbar in the state of introducing 36°C - 38°C hot water into the coating equipment, then switch to 16°C - 18°C cold water, further turn on the turbomolecular pump to pump to a high vacuum below 4.0×10 -5 mbar, and finally conduct a pressure rise test to ensure the normal airtightness of the chamber.
[0018] In the above step S2, the specific method of multiple heating and vacuum pumping is to first set the temperature of the infrared heating tubes to 600°C, heat and keep warm for 45 - 60 minutes, and then pump the vacuum to make the chamber vacuum drop below 4.0×10 -5 mbar; then set the temperature to 550°C again, heat and keep warm for 30 - 45 minutes, and then restore the chamber vacuum to below 4.0×10 -5 mbar to fully remove the moisture and volatile impurities on the surface of the chamber and the substrate.
[0019] In the above step S3, during the etching and cleaning process, the cathode arc round target serving as the ion source uses a Ti target with a diameter of 63mm, a purity of 99.99%, a target current of 75 - 85A, a heating temperature set at 400 - 600°C, a duration of 30 - 60 minutes, and at the same time, the pulsed bias voltage applied to the workpiece substrate is a negative bias voltage of 300V / positive voltage of 20V, the pulse frequency is 20kHz, and the duty cycle is 80%.
[0020] In the above step S4, the target used for sputtering is a rectangular planar TiAlSi alloy target, the elemental composition ratio of the target is 60 at.% Ti, 30 at.% Al, and 10 at.% Si, and the size of the target is 456 mm × 81 mm × 10 mm.
[0021] In the above step S4, the flow rate of nitrogen introduced into the vacuum chamber is 20 sccm, the purity is 99.99%, and the flow rate of argon introduced is 120 sccm, the purity is 99.99%.
[0022] In the above step S4, the infrared electric heating tube is set to a heating temperature of 400 - 600 °C, the average sputtering power of the target is 2 kW - 5 kW, the pulse conduction time is 40 μs, the pulse off time is 1000 μs, and the substrate negative bias voltage is -50 - -200 V; a stepping motor is used to control the rotation speed of the workpiece substrate bracket at 2 rpm - 5 rpm to ensure the uniformity of bracket heating and film coating.
[0023] The present invention has the following advantages and effects compared with the prior art:
[0024] (1) The present invention uses a TiAlSi alloy target, with a stable thin film composition ratio and controllable structure. At the same time, it avoids the pollution of the chamber by introducing silicon source gas and the safety hazards of using dangerous gases. Compared with other multi - element multi - layer coatings, the method of the present invention is simple, safe, and efficient. The TiAlSiN nanocomposite coating suitable for different substrates is prepared by high - power pulsed magnetron sputtering technology. The prepared thin film is uniform and dense, has a low surface roughness, a hardness of more than 40 GPa, a thickness of 1 - 2 μm, and excellent wear and corrosion resistance.
[0025] (2) The present invention adopts an advanced combination technology of arc - enhanced glow discharge technology, pre - ionization, and high - power pulsed magnetron sputtering technology to explore the high - performance process parameter range and realize the controllable preparation of the nano - composite TiAlSiN coating on the substrate surface. Compared with other preparation methods, it not only avoids the large - particle defects left on the substrate surface by arc ion plating but also solves the problem of low metal ionization rate of traditional magnetron sputtering technology. At the same time, the pre - ionization effect brought by arc - enhanced glow discharge is used to optimize the problems of long deposition time and low efficiency in high - power pulsed magnetron sputtering technology. Description of the Drawings
[0026] Figure 1 It is the SEM pattern of the surface of the YG8 cemented carbide substrate, with a magnification of 2000 times.
[0027] Figure 2 It is the SEM pattern of the surface of the YG8 cemented carbide after ion etching and cleaning, with a magnification of 2000 times.
[0028] Figure 3SEM image of the surface of the TiAlSiN film prepared for Example 1, with a magnification of 5000 times.
[0029] Figure 4 EDS spectrum of the TiAlSiN film prepared for Example 1.
[0030] Figure 5 Scratch morphology diagram of the TiAlSiN film prepared for Example 1.
[0031] Figure 6 SEM image of the local scratch morphology of the TiAlSiN film prepared for Example 1, with a magnification of 600 times.
[0032] Figure 7 SEM image of the surface of the YC40 cemented carbide after ion etching and cleaning, with a magnification of 5000 times.
[0033] Figure 8 SEM image of the surface of the TiAlSiN film prepared for Example 2, with a magnification of 5000 times.
[0034] Figure 9 XRD pattern of the TiAlSiN film prepared for Example 2.
[0035] Figure 10 Scratch morphology diagram of the TiAlSiN film prepared for Example 2.
[0036] Figure 11 SEM image of the surface of the TiAlSiN film on the 201 stainless steel substrate prepared for Example 3, with a magnification of 5000 times.
[0037] Figure 12 XRD pattern of the TiAlSiN film prepared for Example 3.
[0038] Figure 13 OM image of the surface of the HRA indentation of the TiAlSiN film prepared for Example 3.
[0039] Figure 14 SEM image of the surface morphology of the TiAlSiN film prepared for Example 3 after electrochemical corrosion, with a magnification of 5000 times.
[0040] Figure 15 Electrochemical polarization curve of the TiAlSiN film prepared for Example 3 in a 3.5 wt% NaCl solution. Detailed implementation manners
[0041] The present invention discloses a method for preparing a TiAlSiN nanocomposite film by high-power pulsed magnetron sputtering. The following further describes the present invention in detail with specific examples.
[0042] The equipment used in the preparation of the TiAlSiN nanocomposite film in the present invention: the HI3 PVD deposition equipment of the domino mini multifunctional of Sulzer Metco, Germany.
[0043] Example 1:
[0044] The Ti-Al-Si-N film is prepared on the surface of YG8 cemented carbide by the method of the present invention.
[0045] 1. Target preparation: Select Ti 60 Al 30 Si 10 alloy as the sputtering target, correctly install it into the coating equipment chamber, and clean its surface with a vacuum cleaner.
[0046] 2. Specimen preparation and furnace loading: Hang and clamp the selected cemented carbide substrate with iron wire, place it in absolute ethanol and ultrasonically clean for 20 min, dry it with hot air, fix it on a three-dimensional rotating planetary holder, and finally push it into the cleaned coating equipment chamber and seal the chamber.
[0047] 3. Chamber vacuum pumping and heating: Pump the chamber vacuum to 4.0×10 -5 mbar through a mechanical pump and a molecular turbo pump, then heat and keep warm at a set value of 600 °C for 60 min, restore the vacuum to 4.0×10 -5 mbar and then heat and keep warm at 550 °C for 30 min again. Subsequently, pump the chamber vacuum to 4.0×10 -5 mbar. Through two heating processes and three vacuum pumping processes, remove the moisture and trace gas impurities inside the chamber and on the substrate surface, fully maintain the vacuum and cleanliness of the chamber, and ensure the quality of the subsequent coating.
[0048] 4. Ion etching of the specimen surface: The etching target is a Ti target with a purity of 99.99%. The target current is set to 85 A, the specimen negative bias voltage is set to 300 V, the temperature of the infrared heating tube is set to 500 °C, the rotation speed of the planetary holder is 2 rpm, continuously introduce high-purity Ar into the vacuum chamber, and maintain the gas pressure in the chamber at 1.0×10 -2 mbar. Use the arc-enhanced glow discharge technology to perform Ar ion cleaning and etching on the cemented carbide substrate for 40 min to enhance the bonding strength between the subsequent coating and the substrate and improve the film-forming quality.
[0049] 5. Deposition of Ti-Al-Si-N thin film: Continuously introduce high-purity argon gas and working gas nitrogen with a fixed flow rate into the vacuum chamber. The flow rate of argon gas is 120 sccm, the flow rate of nitrogen gas is 20 sccm, the temperature of the infrared heating tube is set at 600 °C, the rotation speed of the planetary carrier is 2 rpm, the negative bias value of the sample is set at 150 V, a pulsed bias is applied to the target, the duty cycle is 40 / 1000 μs, the average sputtering power is 4 kW, and the coating process lasts for 180 min.
[0050] 6. Chamber cooling and sampling: After step four is completed, use a circulating cold and hot water system to cool the chamber. The cooling water temperature is controlled at 16 - 18 °C. The sample can be taken out after cooling to below 70 °C in a vacuum state, and the Ti-Al-Si-N thin film of the present invention can be obtained on the surface of the substrate.
[0051] The characteristics of the TiAlSiN thin film prepared on the YG8 cemented carbide substrate by the method of Example 1 are characterized as follows:
[0052] 1. Morphology characterization: Figure 1 、 2 Figures 1, 2, and 3 are the morphologies of the YG8 cemented carbide substrate, the cemented carbide substrate after ion etching, and the TiAlSiN thin film prepared by the method of the present invention observed under a scanning electron microscope, respectively. Among them, Figure 2 the etched cemented carbide substrate shown in Figure 1 removes the loose layer and oxide layer on the surface compared with the substrate shown in Figure 3 to avoid the influence of the Co-depletion phenomenon on the subsequent coating quality.
[0053] 2. Composition characterization: Figure 4 is the EDS energy spectrum of the TiAlSiN film prepared in Example 1. Among them, the atomic ratio of nitrogen element content accounts for 50%, and the ratio of the remaining Ti, Al, and Si elements is about 6:3:1 (atomic ratio), which is consistent with the composition of the alloy target used.
[0054] 3. Hardness characterization: Use a nanoindentation instrument to characterize the intrinsic nano-hardness and elastic modulus of the TiAlSiN film. The average value of its nano-hardness is 43.26 GPa and the average value of the elastic modulus is 498.32 GPa obtained by multi-point testing. The thin film prepared by the present invention meets the standard of super-hard (greater than 40 GPa).
[0055] 4. Film-substrate adhesion characterization: Use the scratch method to characterize the film-substrate adhesion performance, set the loading load to 0 - 100 N, and the scratch length to 5 mm. Figure 5 、 6They are the morphology of the overall scratch under an optical microscope and the morphology of the local scratch at the critical failure load when the coating is completely peeled off or cracked under a scanning electron microscope, respectively. It can be seen that the critical failure load of the film is 68.4 N and the film-substrate adhesion is good.
[0056] Example 2:
[0057] A Ti-Al-Si-N film was prepared on the surface of a YC40 cemented carbide turning tool by the method of the present invention
[0058] 1. Target preparation: The same as in Example 1.
[0059] 2. Specimen preparation and furnace loading: The substrate was selected as a YC40 / SPUN1SNUN120408 cemented carbide turning tool (Zhuzhou Diamond), and its large surface was used as the test surface. The rest was the same as in Example 1.
[0060] 3. Chamber evacuation and heating: The same as in Example 1.
[0061] 4. Ion etching of the specimen surface: The same as in Example 1.
[0062] 5. Deposition of the Ti-Al-Si-N film: The substrate negative bias voltage was set to 100 V, and the rest was the same as in Example 1.
[0063] 6. Chamber cooling and sampling: The same as in Example 1.
[0064] The characteristics of the TiAlSiN film prepared on the YC40 cemented carbide substrate by the method of Example 2 are characterized as follows:
[0065] 1. Morphology characterization: Figure 7 、 8 They are the morphologies of the etched substrate of YC40 cemented carbide and the TiAlSiN film prepared by the method of the present invention observed under a scanning electron microscope. Among them, Figure 8 The film shown is uniform, flat, dense, and has no obvious droplet or pit defects.
[0066] 2. Phase characterization: Figure 9 is the XRD pattern of the TiAlSiN coating. In step 5), the negative bias voltage range is 50-200 V. It can be seen that the phase structure of the prepared film is mainly the cubic TiN phase and the TiAlN2 phase, and the TiN phase shows an obvious (200) preferred orientation. The Si element exists in an amorphous form.
[0067] 3. Hardness characterization: A nano-indentation instrument was used to characterize the intrinsic nano-hardness and elastic modulus of the TiAlSiN film. The average value of its nano-hardness was 35.47 GPa and the average value of the elastic modulus was 780.38 GPa obtained by multi-point testing.
[0068] 4. Characterization of film-substrate bonding strength: The scratch method was used to characterize the film-substrate bonding performance. The loading load was set from 0 to 100 N, and the scratch length was 5 mm. Figure 10 Shown is the morphology of the overall scratch under an optical microscope. It can be seen that the critical failure load of the film is 66.4 N, indicating good film-substrate bonding strength.
[0069] Example 3: Preparation of Ti-Al-Si-N film on the surface of 201 stainless steel by the method of the present invention
[0070] 1. Target preparation: The same as in Example 1
[0071] 2. Specimen preparation and furnace loading: The substrate was selected as a 201 stainless steel sheet, and the rest was the same as in Example 1
[0072] 3. Chamber evacuation and heating: The same as in Example 1
[0073] 4. Ion etching of specimen surface: The same as in Example 1
[0074] 5. Deposition of Ti-Al-Si-N film: The same as in Example 1
[0075] 6. Chamber cooling and sampling: The same as in Example 1
[0076] The characterization of each property of the TiAlSiN film prepared on the 201 substrate by the method of Example 3 is as follows:
[0077] 1. Morphology characterization: Figure 11 Shown are the morphologies of the TiAlSiN film prepared on the surface of 201 stainless steel by the method of the present invention observed under a scanning electron microscope. The shown film is uniform, flat, and dense, without obvious droplet and pit defects.
[0078] 2. Phase characterization: Figure 12 Shown is the XRD pattern of the TiAlSiN film on the surface of 201 stainless steel. It can be seen that the matrix stainless steel is in the austenite phase, and the coating is mainly in the TiN phase.
[0079] 3. Hardness characterization: A nanoindentation instrument was used to characterize the intrinsic nano-hardness and elastic modulus of the TiAlSiN film. The average value of its nano-hardness was obtained as 36.87 GPa and the average value of the elastic modulus was 311.95 GPa through multiple-point tests.
[0080] 3. Film-substrate bonding strength characterization: Figure 13 Shown is the morphology of the HRA indentation. The film and the substrate undergo cooperative deformation, without obvious peeling phenomenon. A small amount of circular cracks appear around the indentation, indicating good bonding strength.
[0081] 3. Electrochemical performance characterization: An electrochemical workstation was used to characterize the corrosion resistance of the TiAlSiN coating in a 3.5 wt% NaCl solution. Figure 14SEM image of the coating surface after electrochemical corrosion Figure 15 The electrochemical polarization curve shows that there are a small number of NaCl crystals and pitting corrosion pits on the coating surface, without obvious corrosion products and coating peeling failure, which proves that the high-density structure of the coating in this invention effectively hinders the infiltration of corrosive media and the corrosion of the substrate material, reduces the tendency of corrosion occurrence, significantly improves the corrosion resistance of the coating, and the annual corrosion rate is 8.53x10 -6 mm / y, with excellent corrosion resistance.
[0082] The implementation manners of the present invention are not limited by the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications made without departing from the spirit and principle of the present invention shall be equivalent replacement manners and are all included in the protection scope of the present invention.
Claims
1. A method for preparing TiAlSiN nanocomposite film by high-power pulsed magnetron sputtering, characterized in that The following steps are included: S1, workpiece substrate surface pretreatment and furnace placement: the workpiece substrate to be coated is surface treated, and then the surface treated workpiece substrate is placed in the furnace chamber of the PVD deposition equipment; S2, vacuuming and heating the furnace chamber: seal the chamber of the vacuum furnace chamber, start vacuuming, and evacuate to a background vacuum of 4.0×10 -5 mbar, then the infrared heating tube is turned on for heating, and the workpiece substrate is pre-treated by plasma etching through multiple heating and vacuuming; S3, plasma etching of the workpiece substrate surface: After completing the pretreatment operation in step S2, the arc-enhanced glow discharge is turned on to perform plasma etching and cleaning on the workpiece substrate. High-purity Ar gas is continuously introduced into the chamber to maintain the chamber pressure at 1×10 - 2 mbar, pulse bias voltage is applied on the workpiece substrate; S4, sputtering coating on the workpiece substrate surface: a fixed ratio of high-purity Ar gas and high-purity N2 is introduced into the vacuum chamber, the temperature of the infrared heating tube in the chamber is kept constant, a DC bias is applied to the workpiece substrate, and a high-power pulsed magnetron sputtering is used to apply a pulsed bias to the target material for 180 minutes of coating treatment to deposit a 1-2 μm TiAlSiN nanocomposite hard film; S5, chamber cooling sampling: After the sputtering coating is completed, the circulating hot and cold water in the furnace chamber is switched to 16℃~18℃ cold water to cool the chamber. When the temperature in the vacuum chamber drops below 70℃, the workpiece substrate can be taken out to complete the TiAlSiN film on the surface of the workpiece substrate.
2. The method for preparing TiAlSiN nanocomposite film by high-power pulsed magnetron sputtering according to claim 1, characterized in that: In step S1, the workpiece substrate is subjected to surface treatment, which means that the surface of the workpiece substrate is mirror-finished and the surface roughness Ra value is less than 0.4 μm.
3. The method for preparing TiAlSiN nanocomposite film by high-power pulsed magnetron sputtering according to claim 1, characterized in that: In step S2, the plasma etching pretreatment of the workpiece substrate refers to removing moisture, trace gases and volatile impurities from the workpiece substrate, the support supporting the workpiece substrate, and the interior of the chamber.
4. The method for preparing TiAlSiN nanocomposite film by high-power pulsed magnetron sputtering according to claim 1, characterized in that: In step S2, the infrared heating tube covers the entire rear wall of the chamber to heat the interior of the chamber by thermal radiation. The actual temperature in the chamber is measured by thermocouples on the left front side of the chamber, which are set at the upper, middle and lower measurement points of the chamber.
5. The method for preparing TiAlSiN nanocomposite film by high-power pulsed magnetron sputtering according to claim 1, characterized in that: In step S2, the vacuum is reduced to 4.0×10 -5 mbar, the coating equipment needs to be pumped to 2.0×10 -5 mbar low vacuum, then switch to 16℃~18℃ cold water, and further turn on the turbomolecular pump to high vacuum 4.0×10 -5 mbar, and finally a pressure rise test is performed to ensure that the chamber is sealed properly.
6. The method for preparing TiAlSiN nanocomposite thin film by high-power pulsed magnetron sputtering according to claim 1, characterized in that: In step S2, the method of multiple heating and vacuuming specifically refers to first setting the temperature of the infrared heating tube to 600°C, heating and keeping the temperature for 45 to 60 minutes, and then vacuuming the chamber to reduce the vacuum degree to 4.0×10 -5 mbar; set the temperature to 550℃ again and heat for 30-45min, then restore the chamber vacuum to 4.0×10 -5 mbar or less, fully removing moisture and volatile impurities from the chamber and substrate surface.
7. The method for preparing TiAlSiN nanocomposite film by high-power pulsed magnetron sputtering according to claim 1, characterized in that: In step S3, during the etching and cleaning process, the cathode arc target acting as the ion source adopts a Ti target with a diameter of 63 mm and a purity of 99.99%. The target current is 75-85A, the heating temperature is set to 400-600°C, and the duration is 30-60min. At the same time, the pulse bias applied to the workpiece substrate is a negative bias of 300V / positive voltage of 20V, a pulse frequency of 20kHz, and a duty cycle of 80%.
8. The method for preparing TiAlSiN nanocomposite film by high-power pulsed magnetron sputtering according to claim 1, characterized in that: In step S4, the target material used for sputtering is a rectangular planar TiAlSi alloy target, the target material element composition ratio is 60at.%Ti, 30at.%Al, 10at.%Si, and the target material size is 456mm×81mm×10mm.
9. The method for preparing TiAlSiN nanocomposite film by high-power pulsed magnetron sputtering according to claim 1, characterized in that: In step S4, the nitrogen gas flow rate into the vacuum chamber is 20 sccm, with a purity of 99.99%, and the argon gas flow rate into the vacuum chamber is 120 sccm, with a purity of 99.99%.
10. The method for preparing TiAlSiN nanocomposite film by high-power pulsed magnetron sputtering according to claim 1, characterized in that: In step S4, the heating temperature of the infrared electric heating tube is set to 400-600°C, the average power of the target sputtering is 2kW-5kW, the pulse on time is 40μs, the pulse off time is 1000μs, and the negative bias voltage of the substrate is -50--200V; a stepper motor is used to control the support speed of the workpiece substrate at 2rpm-5rpm to ensure the uniformity of the support heating and coating.
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