High-strength high-conductivity corrosion-resistant antibacterial alloy film and preparation method thereof

Abstract

The application discloses a kind of high-strength high-conductivity corrosion-resistant antibacterial alloy film and preparation method thereof, adopt the mode of magnetron sputtering in TiAlCrSi alloy Incorporate Ag element, by accurately controlling sputtering process parameters, after polishing cleaning and drying on the surface of stainless steel substrate TiAlCrSiAg alloy film is prepared, realize the significant improvement of the conductivity, corrosion resistance and antibacterial performance of film, the film prepared by the method is dense, and is firmly combined with the substrate, showing excellent corrosion resistance and antibacterial capacity, and under the premise of maintaining relatively high strength, the hardness reduction amplitude is small.The preparation method of the application is simple, easy to operate, and low in cost, suitable for the preparation of multifunctional film materials in the fields of electronic devices, micro-electro-mechanical systems and medical devices, and has high industrial application potential.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of metal surface modification, and particularly relates to a high-strength high-conductivity corrosion-resistant antibacterial alloy film and a preparation method thereof. BACKGROUND

[0002] In modern industry and high-tech fields, the requirements for multifunctionality and high performance of materials are constantly increasing, especially in the electronics, medical, aerospace and other industries. Materials not only need to have high strength and corrosion resistance, but also must have excellent electrical conductivity and antibacterial properties. Traditional alloy materials, although excellent in some properties, are difficult to meet the demand of modern multiple performance. Titanium aluminum chromium silicon (TiAlCrSi) alloy is widely used in the above-mentioned fields due to its stability at high temperature, corrosion resistance and good mechanical properties. However, the deficiency of TiAlCrSi alloy in electrical conductivity and antibacterial property limits its promotion in higher-end applications.

[0003] Silver (Ag) has been widely concerned in the field of material science due to its unique physical and chemical properties, especially excellent electrical conductivity and antibacterial properties. By incorporating Ag into the alloy, the electrical conductivity of the material can be significantly improved, and the material can be endowed with excellent antibacterial properties, making it more suitable for electronic devices, medical devices and harsh environment applications. However, it is a challenge in current material research and development to uniformly incorporate Ag element into alloy film while maintaining its structural integrity and multifunctionality.

[0004] Magnetron sputtering technology has become an ideal choice for the preparation of alloy films because it can precisely control the composition and thickness of the film, and at the same time realize the preparation of high-quality films at low temperature. Currently, there is no related technology report on doping Ag into TiAlCrSi alloy film by magnetron sputtering technology.

[0005] Therefore, it is urgent to develop a technology for preparing Ag-doped TiAlCrSi alloy film by magnetron sputtering method, which has important research and application value for improving the overall performance of materials, prolonging the service life, and improving the safety and reliability of application products. SUMMARY

[0006] The application aims to provide a high-strength high-conductivity corrosion-resistant antibacterial alloy film and a preparation method thereof. By means of magnetron sputtering technology, Ag elements are doped into a TiAlCrSi alloy film, so that the electrical conductivity and antibacterial property of the film can be significantly improved while the high strength and corrosion resistance of the film are ensured. The doped Ag can not only enhance the electronic conduction performance of the film, but also endow the film with persistent antibacterial effect by releasing Ag ions. The multifunctional TiAlCrSiAg alloy film has a wide application prospect in medical devices, electronic components and corrosive environments. The application solves the problems of low hardness, poor corrosion resistance and poor antibacterial property of conventional alloy films.

[0007] In order to achieve the above-mentioned purpose, the application adopts the following technical scheme:

[0008] In the first aspect, the application provides a preparation method of a high-strength high-conductivity corrosion-resistant antibacterial alloy film, comprising the following steps:

[0009] Step 1: The surface of the test piece substrate is polished, and then ultrasonic cleaning is performed. The cleaning reagents are acetone, anhydrous ethanol and deionized water in sequence. After drying, the test piece substrate is ready for use.

[0010] Step 2: Four kinds of pure metal fan-shaped target materials of Ti, Al, Cr and Si are prepared according to the required proportions. The target materials are spliced into a TiAlCrSi alloy target material by means of splicing.

[0011] Step 3: The test piece substrate treated in step 1 is placed in the magnetron sputtering cavity of a magnetron sputtering device. The TiAlCrSi alloy target material and the Ag target material spliced in step 2 are installed on the corresponding target positions in the magnetron sputtering cavity. Then, the magnetron sputtering cavity is vacuumized, and argon gas is introduced into the magnetron sputtering cavity to perform ion etching treatment on the surface of the test piece substrate.

[0012] Step 4: After the magnetron sputtering cavity reaches the predetermined pressure, the TiAlCrSi alloy target material is first opened alone for a period of time, and then the TiAlCrSi alloy target material is closed and the Ag target material is continuously opened. Then, the TiAlCrSi alloy target material is opened for a period of time, and then the TiAlCrSi alloy target material is closed. This process is repeated several times, and the interval time decreases in sequence each time. Finally, the TiAlCrSi alloy target material and the Ag target material are closed to end the film deposition.

[0013] Step 5: After the film deposition is completed, the sample is taken out after the magnetron sputtering cavity is cooled to room temperature, and a high-strength high-conductivity corrosion-resistant antibacterial TiAlCrSiAg alloy film is obtained.

[0014] As a specific technical scheme of the present application, the thickness of the TiAlCrSiAg alloy film is 3.5-4.2 microns.

[0015] As a specific technical scheme of the present application, in step 1, the test piece substrate is any one of iron and its alloys.

[0016] As a specific technical scheme of the present application, in step 1, the test piece substrate is sequentially cleaned with acetone, anhydrous ethanol and deionized water for 10-15 minutes each, and dried at 70-80°C.

[0017] As a specific technical scheme of the present application, in step 2, the TiAlCrSi alloy target has a composition ratio of Ti:Al:Cr:Si = 30:30:30:10, and a purity of no less than 99.90 wt.%; in step 3, the Ag target has a purity of no less than 99.99 wt.%. Specifically, the target is spliced by Ti pieces, Al pieces, Cr pieces and Si pieces with a certain top angle.

[0018] As a specific technical scheme of the present application, in step 3, the TiAlCrSi alloy target is powered by a direct current, and the Ag target is powered by a HiPIMS power source.

[0019] As a specific technical scheme of the present application, in step 3, the magnetron sputtering cavity is vacuumized to a vacuum degree of 1.8x10 -3 Pa-2.7x10 -3 Pa.

[0020] As a specific technical scheme of the present application, in step 3, when argon is introduced for ion etching, the argon flow rate is 50-60 sccm, the argon purity is no less than 99.99%, and the total ion etching time is 10 minutes.

[0021] As a specific technical scheme of the present application, in step 4, the power of the TiAlCrSi alloy target is set to 200-240 W, and the power of the Ag target is set to 400-500 W.

[0022] As a specific technical scheme of the present application, in step 4, the deposition time of the TiAlCrSi alloy target material is opened alone for deposition coating is 70min~100min; the TiAlCrSi alloy target material is opened after the Ag target material is opened for 18min~22min, the power of the TiAlCrSi alloy target material remains unchanged, the deposition time is 18min~22min, then the TiAlCrSi alloy target material is closed; after 12min~17min, the TiAlCrSi alloy target material is opened again, the power of the TiAlCrSi alloy target material remains unchanged, the deposition time is 12min~17min, then the TiAlCrSi alloy target material is closed; after 8min~11min, the TiAlCrSi alloy target material is opened again, the power of the TiAlCrSi alloy target material remains unchanged, the deposition time is 8min~11min, then the TiAlCrSi alloy target material is closed; after 4min~6min, the TiAlCrSi alloy target material is opened again, the power of the TiAlCrSi alloy target material remains unchanged, the deposition time is 4min~6min, then the TiAlCrSi alloy target material is closed.

[0023] In a second aspect, the present application also provides a high-strength high-conductivity corrosion-resistant antibacterial alloy film prepared by the above preparation method.

[0024] Compared with the prior art, the present application provides a high-strength high-conductivity corrosion-resistant antibacterial alloy film and a preparation method thereof, which has the following beneficial effects:

[0025] The high-strength high-conductivity corrosion-resistant antibacterial alloy film and the preparation method thereof provided by the present application adopt a magnetron sputtering method to incorporate Ag elements into the TiAlCrSi alloy, and by accurately controlling the sputtering process parameters, a TiAlCrSiAg alloy film is prepared on the surface of a stainless steel substrate, so that the conductivity, corrosion resistance and antibacterial performance of the film are significantly improved. The film prepared by this method has a dense structure, good bonding effect with the substrate, excellent corrosion resistance and antibacterial capacity, and a small reduction in hardness under the premise of maintaining a high strength.

[0026] The preparation method of the present application is simple, easy to operate and low in cost. The high-strength high-conductivity corrosion-resistant antibacterial alloy film prepared by this method can be used in the fields of electronic devices, micro-electro-mechanical systems and medical devices, and has the prospect of industrial application and commercial production; at the same time, it also has important research and application value in improving the overall performance of materials, prolonging the service life and improving the safety and reliability of application products. BRIEF DESCRIPTION OF DRAWINGS

[0027] In order to make the technical solutions of the embodiments of the present application or the prior art clearer, the accompanying drawings needed in the embodiments or the prior art description will be briefly introduced. Obviously, the accompanying drawings in the following description only represent some of the embodiments of the present application, and all other embodiments obtained by those of ordinary skill in the art without any creative effort based on these accompanying drawings also belong to the protection scope of the present application.

[0028] Figure 1 A cross-sectional view of the TiAlCrSiAg alloy thin film in Example 1;

[0029] Figure 2 A light microscope view of the TiAlCrSiAg alloy thin film after scratch test in Example 1;

[0030] Figure 3 An electrochemical polarization curve view of the TiAlCrSiAg alloy thin film prepared in Examples 1-3 and Comparative Example 1;

[0031] Figure 4 A resistivity / hardness relationship view of the TiAlCrSiAg alloy thin film prepared in Examples 1-3 and Comparative Example 1;

[0032] Figure 5 A plate culture photo of E. coli and Staphylococcus aureus on the TiAlCrSiAg alloy thin film in Example 1;

[0033] Figure 6 A surface antibacterial rate column chart of E. coli and Staphylococcus aureus on the TiAlCrSiAg alloy thin film prepared in Examples 1-3 and Comparative Example 1. DETAILED DESCRIPTION

[0034] The technical solutions of the present application will be described clearly and completely below. Obviously, the described embodiments only represent some of the embodiments of the present application, but not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without any creative effort belong to the protection scope of the present application.

[0035] In the embodiments and comparative examples, the experimental methods used are conventional methods, and the materials, reagents, etc. used are commercially available unless otherwise specified. The equipment and instruments used are conventional prior art equipment and instruments unless otherwise specified.

[0036] The present application will be described in further detail below through detailed embodiments and in conjunction with the accompanying drawings.

[0037] Example 1

[0038] The embodiment provides a high-strength high-conductivity corrosion-resistant antibacterial TiAlCrSiAg alloy film, and a specific preparation method comprises the following steps.

[0039] Step 1: the surface of the 304 stainless steel substrate is subjected to polishing treatment, and then the 304 stainless steel substrate is sequentially placed into ultrasonic tanks respectively containing acetone, anhydrous ethanol and deionized water, and is subjected to ultrasonic cleaning for 12 min in each ultrasonic tank, and then is dried by using an electric hair dryer at a temperature of about 70 DEG C, and is prepared.

[0040] Step 2: according to the proportion of required components, four kinds of pure metal fan-shaped target materials of Ti, Al, Cr and Si are prepared, and various target materials are spliced into a TiAlCrSi alloy target material (purity is not less than 99.90wt.%) by means of splicing target materials, wherein the component proportion of the TiAlCrSi alloy target material is Ti:Al:Cr:Si = 30:30:30:10.

[0041] Step 3: the 304 stainless steel substrate subjected to polishing, cleaning and drying treatment in step 1 is placed in a magnetron sputtering cavity of a magnetron sputtering device, the TiAlCrSi alloy target material and an Ag target material (purity is not less than 99.99wt.%) spliced in step 2 are installed on corresponding target positions in the magnetron sputtering cavity, the TiAlCrSi alloy target material adopts a direct current power supply, and the Ag target material adopts a HiPIMS power supply; then a heating device is opened, the magnetron sputtering cavity is vacuumized to a vacuum degree of about 1.8x10 -3 Pa, and then high-purity argon gas (purity is more than 99.99%) is introduced into the magnetron sputtering cavity to perform ion etching treatment on the surface of the 304 stainless steel substrate, the flow of the introduced argon gas is 50sccm, and the ion etching time is 10 min.

[0042] Step 4: After the predetermined pressure in the magnetron sputtering cavity is reached, the TiAlCrSi alloy target is first opened alone to deposit a film for 80 min, the power of the TiAlCrSi alloy target is set to 200 W, then the TiAlCrSi alloy target is closed and the Ag target is continuously opened, the power of the Ag target is set to 400 W; after 20 min, the TiAlCrSi alloy target is opened, the power of the TiAlCrSi alloy target is adjusted to 200 W, and the deposition is carried out for 20 min, then the TiAlCrSi alloy target is closed; after 15 min, the TiAlCrSi alloy target is opened again, the power of the TiAlCrSi alloy target is adjusted to 200 W, and the deposition is carried out for 15 min, then the TiAlCrSi alloy target is closed; after 10 min, the TiAlCrSi alloy target is opened again, the power of the TiAlCrSi alloy target is adjusted to 200 W, and the deposition is carried out for 10 min, then the TiAlCrSi alloy target is closed; after 5 min, the TiAlCrSi alloy target is opened again, the power of the TiAlCrSi alloy target is adjusted to 200 W, and the deposition is carried out for 5 min, then the TiAlCrSi alloy target and the Ag target are closed, and the film deposition is ended.

[0043] Step 5: After the film deposition is completed, the sample is taken out after the magnetron sputtering cavity is cooled to room temperature, and a high-strength, high-conductivity, corrosion-resistant and antibacterial TiAlCrSiAg alloy film is obtained.

[0044] The prepared TiAlCrSiAg alloy film is subjected to the following detection and characterization, and the results are as shown below:

[0045] (1) The cross-sectional view of the TiAlCrSiAg alloy film is as shown in Figure 1 , and it can be observed that the thickness of the film is 3.61 μm.

[0046] (2) The light microscope view of the prepared TiAlCrSiAg alloy film after scratch test is as shown in Figure 2 , and it can be observed that the film is well combined with the substrate, and the bonding force is 22.49 N.

[0047] (3) The electrochemical polarization curve of the TiAlCrSiAg alloy film is as shown in Figure 3 , and the corrosion current density of the film is 4.293 x 10 -7 A.

[0048] (4) The resistivity / hardness relationship diagram of the TiAlCrSiAg alloy film is as shown in Figure 4 , and the resistivity of the film is 0.81 μΩ / m, and the hardness is 31.67 GPa.

[0049] (5) The bacterial plate culture photo of the TiAlCrSiAg alloy film is as shown inFigure 5 The surface antibacterial rate histogram is shown in Figure 2, and the antibacterial rates are 45.6% (E. coli) and 48.8% (S. aureus). Figure 6

[0050] Example 2

[0051] The embodiment provides a high-strength high-conductivity corrosion-resistant antibacterial TiAlCrSiAg alloy film, and a specific preparation method comprises the following steps:

[0052] Step 1: The surface of the 304 stainless steel substrate is polished, and then the 304 stainless steel substrate is sequentially placed into ultrasonic tanks respectively filled with acetone, anhydrous ethanol and deionized water for ultrasonic cleaning, each ultrasonic tank is subjected to ultrasonic cleaning for 12 min, and then the 304 stainless steel substrate is dried by using an electric hair dryer at a temperature of about 70 DEG C for standby.

[0053] Step 2: Four kinds of pure metal fan-shaped target materials of Ti, Al, Cr and Si are prepared according to the required proportion of ingredients, and the target materials are spliced into a TiAlCrSi alloy target material (the purity is not less than 99.90wt.%) by means of splicing target, wherein the component ratio of the TiAlCrSi alloy target material is Ti:Al:Cr:Si = 30:30:30:10.

[0054] Step 3: The 304 stainless steel substrate subjected to polishing, cleaning and drying treatment in step 1 is placed in a magnetron sputtering cavity of a magnetron sputtering device, the TiAlCrSi alloy target material and an Ag target material (the purity is not less than 99.99wt.%) spliced in step 2 are installed on corresponding target positions in the magnetron sputtering cavity, the TiAlCrSi alloy target material adopts a direct current power supply, and the Ag target material adopts a HiPIMS power supply; then a heating device is turned on, the magnetron sputtering cavity is vacuumized to a vacuum degree of about 1.8x10 -3 Pa, and then high-purity argon gas (the purity is more than 99.99%) is introduced into the magnetron sputtering cavity to perform ion etching treatment on the surface of the 304 stainless steel substrate, the flow rate of the introduced argon gas is 50sccm, and the ion etching time is 10 min.

[0055] ​Step 4: After the predetermined pressure in the magnetron sputtering cavity is reached, the TiAlCrSi alloy target is first opened alone to deposit a film for 80 min, the power of the TiAlCrSi alloy target is set to 200 W, then the TiAlCrSi alloy target is closed and the Ag target is continuously opened, the power of the Ag target is set to 450 W; after 20 min, the TiAlCrSi alloy target is opened, the power of the TiAlCrSi alloy target is adjusted to 200 W, and the deposition is carried out for 20 min, then the TiAlCrSi alloy target is closed; after 15 min, the TiAlCrSi alloy target is opened again, the power of the TiAlCrSi alloy target is adjusted to 200 W, and the deposition is carried out for 15 min, then the TiAlCrSi alloy target is closed; after 10 min, the TiAlCrSi alloy target is opened again, the power of the TiAlCrSi alloy target is adjusted to 200 W, and the deposition is carried out for 10 min, then the TiAlCrSi alloy target is closed; after 5 min, the TiAlCrSi alloy target is opened again, the power of the TiAlCrSi alloy target is adjusted to 200 W, and the deposition is carried out for 5 min, then the TiAlCrSi alloy target and the Ag target are closed, and the film deposition is ended.

[0056] Step 5: After the film deposition is completed, the sample is taken out after the magnetron sputtering cavity is cooled to room temperature, and a high-strength, high-conductivity, corrosion-resistant and antibacterial TiAlCrSiAg alloy thin film is obtained.

[0057] The prepared TiAlCrSiAg alloy thin film is subjected to the following detection and characterization, and the results are as shown below:

[0058] (1) The cross-sectional view of the TiAlCrSiAg alloy thin film is similar to Figure 1 , it can be observed that the thickness of the thin film is 3.76 μm.

[0059] (2) The light microscope view of the prepared TiAlCrSiAg alloy thin film after scratch test is similar to Figure 2 , it can be observed that the thin film is well combined with the substrate, and the bonding force is 20.71 N.

[0060] (3) The electrochemical polarization curve of the TiAlCrSiAg alloy thin film is as shown in Figure 3 , the corrosion current density of the thin film is 4.090 x 10 -7 A.

[0061] (4) The resistivity / hardness relationship diagram of the TiAlCrSiAg alloy thin film is as shown in Figure 4 , the resistivity of the thin film is 0.42 μΩ / m, and the hardness is 29.93 GPa.

[0062] (5) TiAlCrSiAg alloy thin film colony plate culture photo similar Figure 5 The surface antibacterial rate column chart is shown in FIG. 4, and the antibacterial rates are 77.3% (Escherichia coli) and 81.1% (Staphylococcus aureus). Figure 6

[0063] Example 3

[0064] The embodiment provides a high-strength high-conductivity corrosion-resistant antibacterial TiAlCrSiAg alloy thin film, and a specific preparation method comprises the following steps.

[0065] Step 1: The surface of the 304 stainless steel substrate is polished, and then the 304 stainless steel substrate is sequentially placed into ultrasonic tanks respectively filled with acetone, anhydrous ethanol and deionized water for ultrasonic cleaning, each ultrasonic tank is subjected to ultrasonic cleaning for 12 min, and then the 304 stainless steel substrate is dried by using an electric hair dryer at a temperature of about 70 DEG C for standby.

[0066] Step 2: Ti, Al, Cr and Si four kinds of pure metal fan-shaped target materials are prepared according to the proportion of required components, and the target materials are spliced into a TiAlCrSi alloy target material (the purity is not less than 99.90wt.%) by means of splicing target, wherein the component proportion of the TiAlCrSi alloy target material is Ti: Al: Cr: Si = 30: 30: 30: 10.

[0067] Step 3: The 304 stainless steel substrate subjected to polishing, cleaning and drying treatment in step 1 is placed in a magnetron sputtering cavity of a magnetron sputtering device, the TiAlCrSi alloy target material and an Ag target material (the purity is not less than 99.99wt.%) spliced in step 2 are installed on corresponding target positions in the magnetron sputtering cavity, the TiAlCrSi alloy target material adopts a direct current power supply, and the Ag target material adopts a HiPIMS power supply; then a heating device is turned on, the magnetron sputtering cavity is vacuumized to a vacuum degree of about 1.8x10 -3 Pa, and then high-purity argon gas (the purity is more than 99.99%) is introduced into the magnetron sputtering cavity to perform ion etching treatment on the surface of the 304 stainless steel substrate, the flow of the introduced argon gas is 50sccm, and the ion etching time is 10 min.

[0068] ​Step 4: After the predetermined pressure in the magnetron sputtering cavity is reached, the TiAlCrSi alloy target is first opened alone to deposit a film for 80 min, the power of the TiAlCrSi alloy target is set to 200 W, then the TiAlCrSi alloy target is closed and the Ag target is continuously opened, the power of the Ag target is set to 500 W; after 20 min, the TiAlCrSi alloy target is opened, the power of the TiAlCrSi alloy target is adjusted to 200 W, and the deposition is carried out for 20 min, then the TiAlCrSi alloy target is closed; after 15 min, the TiAlCrSi alloy target is opened again, the power of the TiAlCrSi alloy target is adjusted to 200 W, and the deposition is carried out for 15 min, then the TiAlCrSi alloy target is closed; after 10 min, the TiAlCrSi alloy target is opened again, the power of the TiAlCrSi alloy target is adjusted to 200 W, and the deposition is carried out for 10 min, then the TiAlCrSi alloy target is closed; after 5 min, the TiAlCrSi alloy target is opened again, the power of the TiAlCrSi alloy target is adjusted to 200 W, and the deposition is carried out for 5 min, then the TiAlCrSi alloy target and the Ag target are closed, and the film deposition is ended.

[0069] Step 5: After the film deposition is completed, the sample is taken out after the magnetron sputtering cavity is cooled to room temperature, and a high-strength, high-conductivity, corrosion-resistant and antibacterial TiAlCrSiAg alloy thin film is obtained.

[0070] The prepared TiAlCrSiAg alloy thin film is subjected to the following detection and characterization, and the results are as shown below:

[0071] (1) The cross-sectional view of the TiAlCrSiAg alloy thin film is similar Figure 1 , and it can be observed that the thickness of the thin film is 3.88 μm.

[0072] (2) The light microscope view of the prepared TiAlCrSiAg alloy thin film after scratch test is similar Figure 2 , and it can be observed that the combination of the thin film and the substrate is good, and the bonding force is 20.15 N.

[0073] (3) The electrochemical polarization curve of the TiAlCrSiAg alloy thin film is as shown in Figure 3 , the corrosion current density of the thin film is 3.478 x 10 -7 A.

[0074] (4) The resistivity / hardness relationship diagram of the TiAlCrSiAg alloy thin film is as shown in Figure 4 , the resistivity of the thin film is 0.12 μΩ / m, and the hardness is 25.78 GPa.

[0075] (5) The colony plate culture photograph of the TiAlCrSiAg alloy thin film is similar to Figure 5 The surface antibacterial rate column chart is shown in FIG. 3, and the antibacterial rates are 98.7% (Escherichia coli) and 96.9% (Staphylococcus aureus). Figure 6

[0076] Comparative Example 1

[0077] The present comparative example provides a TiAlCrSi alloy thin film, and the specific preparation method comprises the following steps:

[0078] Step 1: The surface of the 304 stainless steel substrate is polished, and then it is sequentially placed in ultrasonic tanks respectively filled with acetone, anhydrous ethanol and deionized water for ultrasonic cleaning, each ultrasonic tank is ultrasonically cleaned for 12 min, and then it is dried with an electric hair dryer at a temperature of about 70°C for standby.

[0079] Step 2: According to the required proportion of ingredients, four kinds of pure metal fan-shaped target materials of Ti, Al, Cr and Si are prepared, and various target materials are spliced into a TiAlCrSi alloy target material (purity not less than 99.90wt.%) by splicing target, wherein the ingredient proportion of the TiAlCrSi alloy target material is Ti:Al:Cr:Si=30:30:30:10.

[0080] Step 3: The 304 stainless steel substrate after polishing, cleaning and drying treatment in step 1 is placed in the magnetron sputtering cavity of the magnetron sputtering device, the TiAlCrSi alloy target material and the Ag target material (purity not less than 99.99wt.%) spliced in step 2 are installed on the corresponding target positions in the magnetron sputtering cavity, the TiAlCrSi alloy target material adopts direct current power supply, and the Ag target material adopts HiPIMS power supply; then the heating device is turned on, the magnetron sputtering cavity is vacuumized to a vacuum degree of about 1.8×10 -3 Pa, and then high-purity argon gas (purity more than 99.99%) is introduced into the magnetron sputtering cavity to perform ion etching treatment on the surface of the 304 stainless steel substrate, the flow rate of the introduced argon gas is 50sccm, and the ion etching time is 10 min.

[0081] Step 4: After the magnetron sputtering cavity reaches the predetermined pressure, the TiAlCrSi alloy target material is deposited and plated for 180 min alone, the power of the TiAlCrSi alloy target material is set to 200W, and then the TiAlCrSi alloy target material is turned off to end the plating.

[0082] Step 5: After the plating is completed, the sample is taken out after the magnetron sputtering cavity is cooled to room temperature, and a TiAlCrSi alloy thin film is obtained.

[0083] ​The prepared TiAlCrSi alloy thin film was detected and characterized as follows, and the results are shown below:

[0084] (1) The cross-sectional view of the TiAlCrSi alloy thin film is similar to that shown in Figure 1 , and it can be observed that the thickness of the thin film is 3.86 μm.

[0085] (2) The optical microscope view of the prepared TiAlCrSi alloy thin film after scratch test is similar to that shown in Figure 2 , and it can be observed that the thin film is well combined with the substrate, and the bonding force is 23.19 N.

[0086] (3) The electrochemical polarization curve of the TiAlCrSi alloy thin film is shown in Figure 3 , and the corrosion current density of the thin film is 7.762 x 10 -6 A.

[0087] (4) The resistivity / hardness relationship diagram of the TiAlCrSi alloy thin film is shown in Figure 4 , and the resistivity of the thin film is 2.54 μΩ / m, and the hardness is 33.15 GPa.

[0088] (5) The bacterial plate culture photo of the TiAlCrSi alloy thin film is similar to that shown in Figure 5 , and the surface antibacterial rate column chart is shown in Figure 6 , and the antibacterial rate is 5.7% (Escherichia coli) and 6.4% (Staphylococcus aureus).

[0089] The above examples only exemplarily illustrate the concepts and technical solutions of the present application, and are not used to limit the present application. Any person skilled in the art can modify or change the above examples without departing from the spirit and scope of the present application. Therefore, all equivalent modifications or changes made by those skilled in the art without departing from the spirit and technical thought of the present application should be covered by the claims of the present application.

[0090] In addition, it should be understood that although the present specification is described in terms of embodiments, each embodiment does not contain only one independent technical solution, and the description manner of the specification is only for clarity, and those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments which can be understood by those skilled in the art.

Claims

1. A method for preparing a high-strength, high-conductivity, corrosion-resistant, and antibacterial alloy film, characterized in that, The method comprises the following steps: Step 1: polishing the surface of the test piece substrate, and then performing ultrasonic cleaning, the cleaning reagents being acetone, anhydrous ethanol and deionized water in sequence, and the test piece substrate being dried and reserved after cleaning; Step 2: preparing Ti, Al, Cr and Si pure metal fan-shaped target materials according to the required proportions, and splicing the target materials into a TiAlCrSi alloy target material through splicing, the component proportion of the TiAlCrSi alloy target material being Ti:Al:Cr:Si=30:30:30:10; Step 3: The substrate of the sample treated in step 1 is placed in a magnetron sputtering cavity of a magnetron sputtering device, and the spliced TiAlCrSi alloy target and the Ag target with a purity of not less than 99.99 wt.% are installed on the corresponding target positions in the magnetron sputtering cavity. The TiAlCrSi alloy target adopts a direct current power supply, and the Ag target adopts a HiPIMS power supply. Then, the magnetron sputtering cavity is vacuumized to a vacuum degree of 1.8×10 -3 Pa~2.7×10 -3 Pa, and then argon gas is introduced into the magnetron sputtering cavity to perform ion etching treatment on the surface of the substrate of the sample. Step 4: setting the power of the TiAlCrSi alloy target material as 200W-240W and the power of the Ag target material as 400W-500W, opening the TiAlCrSi alloy target material alone to deposit a film for 70min-100min after the magnetron sputtering cavity reaches a predetermined pressure, then closing the TiAlCrSi alloy target material and continuously opening the Ag target material, opening the TiAlCrSi alloy target material to deposit a film for 18min-22min after an interval of 18min-22min, then closing the TiAlCrSi alloy target material, opening the TiAlCrSi alloy target material to deposit a film for 12min-17min after an interval of 12min-17min, then closing the TiAlCrSi alloy target material, opening the TiAlCrSi alloy target material to deposit a film for 8min-11min after an interval of 8min-11min, then closing the TiAlCrSi alloy target material, opening the TiAlCrSi alloy target material to deposit a film for 4min-6min after an interval of 4min-6min, then closing the TiAlCrSi alloy target material and the Ag target material to end the film deposition; Step 5: after the film deposition ends, taking out the sample after the magnetron sputtering cavity cools to room temperature, and obtaining the high-strength high-conductivity corrosion-resistant antibacterial TiAlCrSiAg alloy thin film.

2. The production method according to claim 1, characterized by, The thickness of the TiAlCrSiAg alloy thin film is 3.5-4.2um.

3. The preparation method according to claim 1, characterized in that, In step 1, the test piece substrate is any one of iron and its alloys.

4. The production method according to claim 1, characterized by, In step 1, the ultrasonic cleaning time of the test piece substrate using acetone, anhydrous ethanol and deionized water in sequence is 10-15min, and the drying temperature is 70-80℃.

5. The method of claim 1, wherein, In step 3, when the argon gas is introduced for ion etching, the flow rate of the introduced argon gas is 50-60sccm, the purity of the argon gas is higher than 99.99%, and the total ion etching time is 10min.

6. The high-strength, high-conductivity, corrosion-resistant, and antibacterial alloy thin film prepared by the method of any one of claims 1 to 5, characterized in that, The high-strength high-conductivity corrosion-resistant antibacterial alloy thin film is a TiAlCrSiAg alloy thin film.

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