A ti3sic2 max phase coating and method of making the same
By alternating deposition of Ti-Si and Ti-Si-C coatings using high-power pulsed magnetron sputtering technology, combined with vacuum annealing, the problem of preparing high-purity Ti3SiC2 MAX phase coatings at low temperatures was solved, achieving good corrosion resistance and film-substrate adhesion in high-humidity and high-salt marine environments.
Patent Information
- Application Number
- CN202410404770.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-07
- Publication Date
- 2026-05-15
- Estimated Expiration
- 2044-04-07
AI Technical Summary
Existing technologies make it difficult to prepare high-purity Ti3SiC2 MAX phase coatings at low temperatures, and the coatings are prone to corrosion in high-humidity and high-salt marine environments, affecting the service performance of compressor blades.
High-power pulsed magnetron sputtering technology was used to alternately deposit Ti-Si and Ti-Si-C coatings, combined with vacuum annealing to control the Ti to Si atomic ratio. Carbon hydride was used as the reaction gas source, and the carbon atom content was controlled during the deposition process to form a high-purity Ti3SiC2 MAX phase coating.
A high-purity Ti3SiC2 MAX phase coating was prepared at a relatively low temperature. The coating exhibits good resistance to salt spray corrosion, and the SiO2 layer provides passivation protection. The coating has a dense structure and strong film-substrate adhesion, making it suitable for various working conditions.
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Figure CN118345336B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of surface strengthening functional coating materials, and in particular to a Ti3SiC2 MAX phase coating and its preparation method. Background Technology
[0002] With increasing performance requirements for marine equipment, the operating temperature of compressor blades in their engines is also rising. The high humidity and salinity of the marine environment can lead to severe corrosion of compressor blades during service. Surface coating protection is an effective measure to improve the performance, reliability, and lifespan of compressor blades under extreme environments and complex operating conditions. Currently, both domestically and internationally, hard coatings such as TiN, CrC, and ZrN are mainly used as erosion-resistant coatings on compressor blades. While these coatings provide good erosion protection in dry air, in the severely humid or salty marine environment at 400–700℃, NaCl + H2O can react chemically with TiO2 in the coating, causing oxide film damage, stress corrosion crack growth, and an increased corrosion rate. NaCl can also react with Cr to form volatile chromium chlorides at high temperatures, resulting in an incomplete oxide film. This weakens the passivating effect of Cr, accelerates coating peeling, and reduces protective performance.
[0003] MAX phases are a class of thermodynamically stable, layered, high-performance ceramic-metal materials with a close-packed hexagonal structure, and their general formula is M. n+1 AX n In a MAX phase, n is typically 1–3, M is a transition metal, A is usually a Group 3 or Group 4 element, and X is C or N. Early MAX phases were classified into three types: 211, 312, and 413. In MAX phases, the electron clouds of M and X atoms overlap, resulting in strong ionic and covalent bonds, while the electron clouds of M and A atoms overlap, resulting in weaker metallic bonds. This unique layered structure and bonding characteristics endow MAX phases with the excellent properties of both metals and ceramics, such as good mechanical stability, high hardness, good thermal shock resistance, excellent corrosion resistance and high-temperature oxidation resistance, good electrical and thermal conductivity, self-healing properties, and machinability. Therefore, they have potential applications in high-tech fields such as nuclear energy, marine engineering, aerospace, and biomedicine.
[0004] Ti3SiC2, the MAX phase in the Ti-Si-C system, exhibits a low electrochemical corrosion rate and high chemical corrosion activation energy under medium-temperature salt spray conditions. It also possesses higher hardness, elastic modulus, flexural strength, and fracture toughness, making it an ideal material for surface protective coatings of nickel-based superalloys and stainless steel under harsh and complex working conditions. However, the 312 MAX phase has a long c-axis in its crystal structure, requiring longer diffusion paths for atoms during phase formation, thus necessitating more energy. Therefore, synthesis often requires sufficiently long times and high temperatures to form a complete crystal structure. Currently, the preparation of Ti3SiC2 coatings requires temperatures exceeding 1000℃, with bulk formation occurring at temperatures as high as 1450–1700℃, limiting its application range. Patent document CN113981392A discloses a low-temperature phase formation preparation method for MAX phase coatings, employing high-power pulsed magnetron sputtering technology to prepare MAX phase coatings, enabling the preparation of Ti3AlC2 312 MAX phases at relatively low heat treatment temperatures. However, because Si atoms in Ti3SiC2 are prone to insertion and extraction, the preparation process often involves a significant amount of TiC and Ti5Si3C. x The formation of impurity phases such as Ti3SiC2MAX generally results in low purity of the obtained Ti3SiC2MAX phase, which affects the coating performance. Summary of the Invention
[0005] In view of the shortcomings of the prior art, the technical problem to be solved by the present invention is how to prepare a high-purity Ti3SiC2 MAX phase coating at a lower temperature.
[0006] To achieve the above objectives, the present invention provides a method for preparing a Ti3SiC2 MAX phase coating, comprising the following steps:
[0007] S1. A Ti-Si transition layer is deposited on the substrate surface using high-power pulsed magnetron sputtering technology;
[0008] S2. Carbon hydride is introduced, and Ti-Si coating and Ti-Si-C coating are deposited alternately, with the number of alternating depositions being 2 to 8 times;
[0009] S3. The prepared coating is subjected to vacuum annealing to obtain a Ti3SiC2 MAX phase coating.
[0010] This invention employs high-power pulsed magnetron sputtering (HiPIMS) technology to alternately deposit Ti-Si and Ti-Si-C coatings. The deposited coatings can form phases at lower temperatures during subsequent heat treatment, and can reduce the generation of impurity phases and improve the purity of the MAX phase.
[0011] Further, step S2 specifically includes: using a Ti-Si alloy target as the sputtering target, employing high-power pulsed magnetron sputtering technology, and alternately depositing Ti-Si and Ti-Si-C coatings on the cleaned substrate surface at a frequency of 500–1000 Hz and a duty cycle of 5–10%, with carbon hydride used as the reaction gas source during Ti-Si-C coating deposition. HiPIMS can apply a high-peak-power unipolar pulse to the cathode, thereby generating a high peak electron density near the target. The lower duty cycle and higher peak power density during high-power discharge of the target improve the ionization rate of the sputtered material, enhance the kinetic energy of particles incident on the substrate surface, and effectively reduce the formation temperature of the MAX phase.
[0012] Furthermore, the Ti to Si atomic ratio of the Ti-Si alloy target is 2:1.5 to 2. Controlling the Ti to Si atomic ratio is beneficial to improving the purity of the MAX phase.
[0013] Furthermore, the flow rate of the reaction gas source is 7–15 sccm. By using carbon hydrides as the reaction gas source to introduce carbon atoms, the carbon atom content in the coating can be flexibly adjusted according to the environmental protection requirements of the coating.
[0014] Furthermore, in step S2, the deposition time of the Ti-Si coating during each alternating deposition process is 5–15 min, and the deposition time of the Ti-Si-C coating is 15–30 min. The alternating deposition forms an alternating structure of Ti-Si and Ti-Si-C coatings, which confines Si atoms, reduces the generation of impurity phases, and improves the MAX phase purity of the coating. Moreover, this coating maintains structural stability after undergoing medium-temperature salt spray corrosion, exhibiting good corrosion resistance.
[0015] Furthermore, in step S3, the annealing temperature is 750–900°C. The heat treatment process of this invention enables phase formation at a lower temperature, reducing the temperature by approximately 200–500°C compared to existing technologies.
[0016] Furthermore, the thickness of the transition layer is 0.5–2 μm, and the thickness of the Ti3SiC2 MAX phase coating is 3–7 μm. A transition layer is deposited on the substrate surface to improve film-substrate adhesion and compatibility, resulting in a dense coating structure with a smooth, defect-free surface.
[0017] Furthermore, in step S1, the sputtering deposition parameters of the transition layer are: sputtering power of 1500-2500W and substrate bias of -150--50V.
[0018] Furthermore, the substrate surface is subjected to plasma glow etching before the deposition of the transition layer. Plasma glow etching of the substrate surface can effectively remove contaminants.
[0019] Furthermore, the gas used in plasma glow etching is argon or nitrogen, and the etching parameters are: plasma flow rate of 29-35 sccm, ion source voltage of 1000-1100 V, substrate bias voltage of -300--150 V, and etching time of 20-60 min.
[0020] The present invention also provides a Ti3SiC2 MAX phase coating, prepared by the above-described method, wherein the Ti3SiC2 MAX phase coating exhibits close-packed hexagonal equiaxed crystal growth. The Ti3SiC2 MAX phase in the coating prepared by the present invention has a purity exceeding 92%, and the prepared coating exhibits strong film-substrate bonding, a dense structure, a smooth and defect-free surface, and excellent resistance to salt spray corrosion.
[0021] In summary, compared with the prior art, the present invention has the following beneficial effects:
[0022] (1) In this invention, Ti-Si coating and Ti-Si-C coating are deposited alternately using high-power pulsed magnetron sputtering (HiPIMS) technology. Ti-Si plays a certain role in limiting the Si atoms in Ti-Si-C. During the subsequent high-temperature heat treatment, C atoms diffuse to form a high-purity Ti3SiC2 MAX phase.
[0023] (2) The MAX phase coating of the present invention has good resistance to salt spray corrosion. Its Si atomic layer is relatively stable. The corrosion layer formed consists of an inner TiO2 layer and an outer SiO2 layer. The chemical inertness of SiO2 enables it to play a good passivation protection role, preventing the corrosive medium from further diffusing inward and accelerating corrosion.
[0024] (3) The present invention uses Ti-Si alloy target and carbon-containing gas as sputtering source, which reduces the number of target materials and facilitates the adjustment of process parameters; and by introducing carbon atoms through gas source, the carbon atom content in the coating can be flexibly adjusted according to the coating protection environment requirements, thereby adjusting the proportion of Ti3SiC2 MAX phase in the coating to meet the actual working conditions. The coating prepared under low gas flow conditions has better toughness, and the coating prepared under high gas flow conditions has higher hardness.
[0025] (4) The present invention utilizes a high-power pulsed power supply to sputter the target material. HiPIMS can apply a high peak power unipolar pulse to the cathode, thereby generating a high peak electron density near the target material, which is three orders of magnitude higher than that of DC magnetron sputtering technology (DCMS). The lower duty cycle and higher peak power density in the high-power discharge of the target material improve the ionization rate of the sputtered material, enhance the dynamic energy of the particles incident on the substrate surface, effectively reduce the phase formation temperature of the MAX phase, and enable the deposited Ti-Si-C coating to form a phase at a lower temperature during the subsequent heat treatment process.
[0026] (5) The present invention first deposits a Ti-Si transition layer on the substrate surface, and then deposits an alternating coating layer, which can improve the coating film-substrate bonding force, make the coating structure dense, and make the surface smooth and defect-free. Attached Figure Description
[0027] Figure 1 The images show the XRD patterns of the Ti3SiC2 MAX phase coatings prepared in Examples 1, 2, and 3 of this invention.
[0028] Figure 2 This is a SEM image of the surface morphology of the Ti3SiC2 MAX phase coating prepared in Example 1 of the present invention.
[0029] Figure 3 These are SEM images of the cross-sectional morphology of the Ti3SiC2 MAX phase coating prepared in Example 3 of this invention, and EDS linear distribution diagrams of cross-sectional elements.
[0030] Figure 4 The image shows the XRD pattern of the Ti3SiC2 MAX phase coating prepared in Example 3 of this invention after a salt spray corrosion experiment.
[0031] Figure 5 This is a SEM image of the surface morphology of the Ti3SiC2 MAX phase coating prepared in Example 3 of the present invention after a salt spray corrosion experiment.
[0032] Figure 6 These are the XRD patterns of the Ti3SiC2 MAX phase coatings prepared by Comparative Examples 1, 2, and 3 of this invention after annealing.
[0033] Figure 7 This is a SEM image of the surface morphology of the Ti3SiC2 MAX phase coating prepared as described in Comparative Example 3 of the present invention after a salt spray corrosion experiment. Detailed Implementation
[0034] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
[0035] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Every smaller range between any stated value or intermediate value within a stated range, and any other stated value or intermediate value within said range, is also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.
[0036] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be readily apparent to those skilled in the art.
[0037] This invention provides a Ti3SiC2 MAX phase coating and its preparation method. High-power pulsed magnetron sputtering technology is used. First, a Ti-Si transition layer is deposited on the substrate surface. Then, Ti-Si coatings and Ti-Si-C coatings are alternately deposited on the transition layer. The prepared coatings are then vacuum annealed to obtain a high-purity Ti3SiC2 MAX phase coating. The substrate material can be selected from nickel-based alloys, titanium alloys, stainless steel, etc. The deposited Ti-Si-C coating exhibits columnar crystal growth, while the MAX phase coating exhibits close-packed hexagonal equiaxed crystal growth. The specific steps of the preparation method are as follows:
[0038] S0. Substrate surface cleaning. Plasma glow etching is performed using argon or nitrogen gas. The plasma glow etching parameters are: plasma flow rate of 29–35 sccm, ion source voltage of 1000–1100 V, substrate bias voltage of -300–-150 V, and etching time of 20–60 min.
[0039] S1. Deposition of the transition layer. A Ti-Si transition layer is deposited on the substrate surface using high-power pulsed magnetron sputtering with a Ti-Si alloy target. The Ti-Si atomic ratio of the Ti-Si alloy target is 2:1.5–2. Before deposition, the deposition chamber is heated to 150–300°C, and an inert protective gas is introduced at a flow rate of 150–250 sccm. The sputtering parameters for the transition layer are: sputtering power of 1500–2500 W, and a bias voltage applied to the substrate of -150–-50 V. Preferably, the thickness of the transition layer is 0.5–2 μm.
[0040] S2. Alternating Deposition of Coatings. Using a Ti-Si alloy target as the sputtering target, high-power pulsed magnetron sputtering technology was employed to alternately deposit Ti-Si and Ti-Si-C coatings on the cleaned substrate surface at a frequency of 500–1000 Hz and a duty cycle of 5–10%. During the deposition of the Ti-Si-C coating, carbon hydride was used as the reaction gas source, with methane or acetylene as the hydride, and a flow rate of 7–15 sccm. The deposition time for each Ti-Si coating was 5–15 min, and the deposition time for the Ti-Si-C coating was 15–30 min, resulting in a coating thickness of 3–7 μm.
[0041] S3. Vacuum annealing. The prepared coating is placed in an annealing furnace, with the vacuum level inside the furnace below 3 × 10⁻⁶ before heating begins. -3The annealing heat treatment temperature was 750-900℃, and the time was 60-180min. After vacuum annealing, a Ti3SiC2 MAX phase coating was obtained.
[0042] The above method can prepare a high-purity Ti3SiC2 MAX phase coating at a relatively low temperature. The prepared coating has a dense structure, a smooth and defect-free surface, and maintains structural stability after being subjected to medium-temperature salt spray corrosion, thus exhibiting excellent corrosion resistance.
[0043] The technical effects of the present invention will be described below with reference to specific embodiments.
[0044] Example 1
[0045] In this embodiment, the substrate material is Inconel 718 nickel-based alloy, and the specific preparation method of the Ti3SiC2 MAX phase coating on the substrate surface is as follows:
[0046] (1) Use silicon carbide metallographic sandpaper to grind the Inconel 718 nickel-based alloy substrate from low to high grit up to 3000#, and then use diamond polishing compound to polish it to a mirror finish. Clean the polished substrate with acetone and ethanol for 15 minutes each, and after air drying, use conductive adhesive to attach the substrate to the frame and place it in the deposition chamber.
[0047] (2) Set the deposition chamber temperature to 200℃, and wait for the chamber vacuum to reach 3×10. -5 When the Torr is below 0, 32 sccm of high-purity argon gas is introduced into the vacuum deposition chamber, the linear anolyte ion source current is set to 0.2A and a bias voltage of -200V is applied to the substrate, and the surface of the Inconel 718 nickel-based alloy substrate is cleaned by argon plasma glow discharge etching for 30 minutes.
[0048] (3) A Ti-Si transition layer was deposited on the surface of the Inconel 718 nickel-based alloy substrate after etching and cleaning using high-power pulsed magnetron sputtering technology. 200 sccm of high-purity argon gas was introduced into the chamber, the substrate bias voltage was adjusted to -50V, the sputtering target was an alloy target with a Ti-Si atomic ratio of 1:1, the HiPIMS power supply frequency was set to 500Hz, the period was 2000μs, the duty cycle was 5%, the power applied to the sputtering target during the deposition process was kept constant at 2000W, and the Ti-Si transition layer deposition time was 30min.
[0049] (4) A Ti-Si layer was first deposited on the surface of the transition layer for 10 min using high-power pulsed magnetron sputtering technology. Then, 10 sccm of high-purity methane reaction gas was introduced to provide carbon atoms for the deposition of a Ti-Si-C layer for 20 min. This process was repeated 4 times.
[0050] (5) Place the deposited sample in a tube furnace and wait for the vacuum level to reach 1×10. -3 When the temperature is below Pa, the sample is heated to 850℃ at a heating rate of 10℃ / min and held at this temperature for 90min. Then it is naturally cooled to room temperature to obtain the Ti3SiC2MAX coating.
[0051] Example 2
[0052] In this embodiment, the substrate material is 1Cr11Ni2W2MoV stainless steel, and the specific preparation method of the Ti3SiC2 MAX phase coating on the substrate surface is as follows:
[0053] (1) Use silicon carbide metallographic sandpaper to grind the 1Cr11Ni2W2MoV stainless steel substrate from low to high grit up to 3000#, and then use diamond polishing agent to polish it to mirror finish. Clean the polished substrate with acetone and ethanol for 15 minutes each, and after air drying, use conductive adhesive to attach the substrate to the frame and place it in the deposition chamber.
[0054] (2) Set the deposition chamber temperature to 200℃, and wait for the chamber vacuum to reach 3×10. -5 When the Torr is below 0, 32 sccm of high-purity argon gas is introduced into the vacuum deposition chamber, the linear anodic ion source current is set to 0.2A and a bias voltage of -200V is applied to the substrate, and the surface of the 1Cr11Ni2W2MoV stainless steel substrate is cleaned by argon plasma glow discharge etching for 30 minutes.
[0055] (3) A Ti-Si transition layer was deposited on the surface of a 1Cr11Ni2W2MoV stainless steel substrate after etching and cleaning using high-power pulsed magnetron sputtering technology. 200 sccm of high-purity argon gas was introduced into the chamber, the substrate bias voltage was adjusted to -50V, the sputtering target was an alloy target with a Ti-Si atomic ratio of 1:1, the HiPIMS power supply frequency was set to 500Hz, the period was 2000μs, the duty cycle was 5%, the power applied to the sputtering target during the deposition process was kept constant at 2000W, and the Ti-Si transition layer deposition time was 30min.
[0056] (4) A Ti-Si layer was first deposited on the surface of the transition layer for 5 min using high-power pulsed magnetron sputtering technology. Then, 10 sccm of high-purity methane reaction gas was introduced to provide carbon atoms for the deposition of a Ti-Si-C layer for 15 min. This process was repeated 8 times.
[0057] (5) Place the deposited sample in a tube furnace and wait for the vacuum level to reach 1×10. -3 When the temperature is below Pa, the sample is heated to 850℃ at a heating rate of 10℃ / min and held at this temperature for 90min. Then it is naturally cooled to room temperature to obtain the Ti3SiC2MAX coating.
[0058] Example 3
[0059] In this embodiment, TC4 titanium alloy is selected as the substrate material, and the specific preparation method of the Ti3SiC2 MAX phase coating on the substrate surface is as follows:
[0060] (1) Use silicon carbide metallographic sandpaper to grind the TC4 titanium alloy substrate from low to high grit up to 3000#, and then use diamond polishing agent to polish it to a mirror finish. Clean the polished substrate with acetone and ethanol for 15 minutes each, and after air drying, use conductive adhesive to attach the substrate to the frame and place it in the deposition chamber.
[0061] (2) Set the deposition chamber temperature to 200℃, and wait for the chamber vacuum to reach 3×10. -5 When the Torr is below 0, 32 sccm of high-purity argon gas is introduced into the vacuum deposition chamber, the linear anodic ion source current is set to 0.2A and a bias voltage of -200V is applied to the substrate, and the surface of the TC4 titanium alloy substrate is cleaned by argon plasma glow etching for 30 minutes.
[0062] (3) A Ti-Si transition layer was deposited on the surface of the etched and cleaned TC4 titanium alloy substrate using high-power pulsed magnetron sputtering technology. 200 sccm of high-purity argon gas was introduced into the chamber, the substrate bias voltage was adjusted to -50V, the sputtering target was an alloy target with a Ti-Si atomic ratio of 1:1, the HiPIMS power supply frequency was set to 500Hz, the period was 2000μs, the duty cycle was 5%, the power applied to the sputtering target during the deposition process was kept constant at 2000W, and the Ti-Si transition layer deposition time was 30min.
[0063] (4) A Ti-Si layer was first deposited on the surface of the transition layer for 15 min using high-power pulsed magnetron sputtering technology. Then, 10 sccm of high-purity methane reaction gas was introduced to provide carbon atoms for the deposition of a Ti-Si-C layer for 25 min. This process was repeated three times.
[0064] (5) Place the deposited sample in a tube furnace and wait for the vacuum level to reach 1×10. -3 When the temperature is below Pa, the sample is heated to 850℃ at a heating rate of 10℃ / min and held at this temperature for 90min. Then it is naturally cooled to room temperature to obtain the Ti3SiC2MAX coating.
[0065] The Ti3SiC2 MAX coatings prepared in Examples 1, 2, and 3 were characterized, and their XRD patterns are shown below. Figure 1 As shown, the coating is mainly composed of Ti3SiC2, and the MAX phase has high purity.
[0066] The surface morphology of the Ti3SiC2 MAX coating prepared in Example 1 is as follows: Figure 2 As shown, the coating structure is dense and the surface is smooth and free of defects.
[0067] Figure 3 The cross-sectional morphology SEM image of the Ti3SiC2 MAX phase coating prepared in Example 3 is shown, which shows that the coating and the substrate are tightly bonded and the film-substrate bonding is good.
[0068] Figure 4 and Figure 5 The XRD patterns and surface morphology images of the Ti3SiC2 MAX phase coating prepared in Example 3 after a salt spray corrosion test at 750℃ for 12h are shown respectively. It can be seen that the coating is still dominated by Ti3SiC2 MAX after corrosion, basically maintaining the phase composition before corrosion. Moreover, the surface morphology is intact after corrosion without peeling, showing good salt spray corrosion resistance.
[0069] Comparative Example 1
[0070] The difference between this comparative example and Example 1 is that in step (4), a Ti-Si-C coating is directly deposited for 60 min without alternating deposition. Otherwise, the other steps of the preparation method of the substrate and the Ti3SiC2 MAX phase coating on the substrate surface are the same as those in Example 1.
[0071] Comparative Example 2
[0072] The difference between this comparative example and Example 3 is that no Ti-Si transition layer was deposited after plasma etching and before the Ti-Si-C coating was deposited. Otherwise, the other steps of the preparation method of the substrate and the Ti3SiC2 MAX phase coating on the substrate surface are the same as those in Example 3.
[0073] Comparative Example 3
[0074] The difference between this comparative example and Example 3 is that DC magnetron sputtering was used to prepare the Ti-Si-C coating. Other than that, the other steps of the preparation method of the substrate and the Ti3SiC2 MAX phase coating on the substrate surface are the same as those in Example 3.
[0075] The Ti3SiC2 MAX coatings prepared in Comparative Examples 1, 2, and 3 were characterized, and their XRD patterns are shown below. Figure 6 As shown, the content of Ti3SiC2MAX phase in the coating is low, and it is mainly composed of impurity phases such as TiC and Ti5Si3.
[0076] Figure 7The surface morphology of the Ti3SiC2 MAX coating prepared in Comparative Example 3 after salt spray corrosion at 750℃ for 12h is shown. It can be seen that the surface of the coating is rough and partially peeled off after corrosion, indicating poor corrosion performance.
[0077] While the present invention has been disclosed above, its scope of protection is not limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of this disclosure, and all such changes and modifications will fall within the scope of protection of this invention.
Claims
1. A method for preparing a Ti3SiC2 MAX phase coating, characterized in that, Includes the following steps: S1. A Ti-Si transition layer is deposited on the substrate surface using high-power pulsed magnetron sputtering technology; S2. Carbon hydride is introduced, and Ti-Si coating and Ti-Si-C coating are deposited alternately, with the number of alternating depositions being 2 to 8 times; S3. The prepared coating is subjected to vacuum annealing at a temperature of 750–900 °C to obtain a Ti3SiC2 MAX phase coating.
2. The method for preparing the Ti3SiC2 MAX phase coating according to claim 1, characterized in that, Step S2 specifically includes: using a Ti-Si alloy target as the sputtering target, employing high-power pulsed magnetron sputtering technology, and alternately depositing Ti-Si coatings and Ti-Si-C coatings on the cleaned substrate surface at a frequency of 500-1000Hz and a duty cycle of 5-10%, with carbon hydrides used as the reaction gas source when depositing the Ti-Si-C coating.
3. The method for preparing the Ti3SiC2 MAX phase coating according to claim 2, characterized in that, The Ti-Si alloy target has a Ti to Si atomic ratio of 2:1.5 to 2.
4. The method for preparing the Ti3SiC2 MAX phase coating according to claim 3, characterized in that, The flow rate of the reaction gas source is 7–15 sccm.
5. The method for preparing the Ti3SiC2 MAX phase coating according to claim 4, characterized in that, In step S2, the deposition time of the Ti-Si coating during each alternating deposition process is 5 to 15 minutes, and the deposition time of the Ti-Si-C coating is 15 to 30 minutes.
6. The method for preparing the Ti3SiC2 MAX phase coating according to claim 1, characterized in that, The thickness of the transition layer is 0.5–2 μm, and the thickness of the Ti3SiC2 MAX phase coating is 3–7 μm.
7. The method for preparing the Ti3SiC2 MAX phase coating according to claim 1, characterized in that, In step S1, the sputtering deposition parameters for the transition layer are: sputtering power of 1500-2500W and substrate bias of -150--50V.
8. The method for preparing the Ti3SiC2 MAX phase coating according to claim 1, characterized in that, Plasma glow lithography was performed on the substrate surface before the deposition of the transition layer.
9. A Ti3SiC2 MAX phase coating, characterized in that, The coating is prepared by any one of the preparation methods described in claims 1 to 8, and the coating exhibits close-packed hexagonal equiaxed crystal growth.