A method for preparing a coating on the surface of an ultrasonic scalpel by magnetron sputtering

Abstract

This invention discloses a method for preparing a coating on the surface of an ultrasonic surgical scalpel by magnetron sputtering. The substrate of the ultrasonic surgical scalpel is made of titanium alloy. The method includes the following steps: S1. Pretreatment of the substrate surface; S2. Loading: The pretreated substrate from step S1 is mounted on a sample rotating frame and placed into a magnetron sputtering deposition chamber; S3. Glow photoluminescence cleaning: The substrate is subjected to plasma glow photoluminescence cleaning; S4. Preparation of intermediate coating: An intermediate Al coating is prepared by magnetron sputtering using Al target material as sputtering raw material and Ar gas as sputtering gas; S5. Coating preparation: An AlN-Al coating is prepared on the intermediate Al coating by magnetron sputtering using both Al and AlN targets as sputtering raw materials and Ar gas as sputtering gas. The Al mass fraction content in the AlN-Al coating is 1%-2%. This invention uses an Al transition layer as an intermediate layer between the coating and the substrate, solving the problem of bonding strength between the two; the doping of Al element in the thin film successfully solves the problem of high friction coefficient of AlN coating.

Description

Technical Field

[0001] This invention relates to a method for preparing a coating on the surface of an ultrasonic surgical scalpel by magnetron sputtering, belonging to the field of titanium alloy surface coating preparation technology. Background Technology

[0002] TC4 titanium alloy, or Ti-6Al-4V, is an alloy material widely used in biomedical engineering, petrochemicals, aerospace, and other fields. It possesses advantages such as low density, high strength, good toughness and thermoplasticity, and good biocompatibility. However, in practical applications, the poor frictional properties of titanium alloys lead to significant wear, making them unable to resist wear caused by the frictional behavior of moving parts. Furthermore, the surface of titanium alloys exhibits adhesion, making them difficult to adapt to complex service conditions. These defects affect its practical application, causing significant energy loss and limiting its industrial application range.

[0003] To adapt materials to various special environments, a coating is often deposited on the material surface. Various surface physical and chemical treatment methods can impart desired properties to materials that they do not possess otherwise. Therefore, surface modification of titanium alloys is the best approach, achieving both excellent surface physical and mechanical properties and friction characteristics while retaining the inherent advantages of titanium alloys.

[0004] Electroplating technology is widely used, but it pollutes the environment and poses a threat to human health. Hot-dip galvanizing produces a thicker but less uniform coating than electroplating and generates a large amount of waste gas, causing environmental pollution. Thermal spraying coatings use a wide range of materials, essentially capable of spraying all engineering solid materials. However, the bonding strength between the thermally sprayed coating and the substrate is not high, and the coating's impact resistance and heavy-duty performance are poor. When manual operation of thermal spraying technology is required, the environment is generally harsh, with problems such as noise, dust, high heat, and radiation. Chemical vapor deposition technology has a relatively low deposition rate, is difficult to operate, and is not conducive to mass production. Therefore, it is necessary to invent a preparation method that meets performance requirements, complies with green environmental protection requirements, is simple to operate, has good repeatability, and is convenient for industrial production and application. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides a method for preparing a coating on the surface of an ultrasonic surgical scalpel using magnetron sputtering. The specific technical solution is as follows.

[0006] A method for preparing a coating on the surface of an ultrasonic surgical scalpel by magnetron sputtering, wherein the substrate of the ultrasonic surgical scalpel is made of titanium alloy, characterized by comprising the following steps:

[0007] S1. Pre-treatment of the substrate surface: grinding, polishing, ultrasonic cleaning, and drying the substrate;

[0008] S2. Loading: The pretreated substrate from step S1 is mounted on the sample rotating frame and placed into the magnetron sputtering coating chamber;

[0009] S3. Glow Glow Cleaning: Perform plasma glow cleaning on the substrate for 15-20 minutes, while simultaneously starting the heater to heat the pre-coated sample.

[0010] S4. Preparation of intermediate coating: Using Al target as sputtering raw material and Ar gas as sputtering gas, the intermediate Al coating is prepared by magnetron sputtering.

[0011] S5. Coating preparation: Using Al and AlN targets as sputtering raw materials and Ar gas as sputtering gas, an AlN-Al coating is prepared on the intermediate Al coating by magnetron sputtering. The mass fraction of Al in the AlN-Al coating is 1%-2%.

[0012] Preferably, the matrix material is a Ti-6Al-4V titanium alloy.

[0013] Preferably, in step S1, the substrate is successively polished with 400-grit, 800-grit, 1500-grit, and 2000-grit sandpaper, then polished on a polishing machine, then cleaned with acetone degreasing agent for 40 minutes, ultrasonically cleaned with pure water for 40 minutes, and finally dried with an air gun.

[0014] Preferably, in step S2, the distance between the substrate surface and the target position is 9-11 cm.

[0015] Preferably, step S3 includes: evacuating to a vacuum of 1×10⁻⁶. -3 Pa, open the Ar gas cylinder to fill the vacuum membrane cavity with Ar gas, adjust the flow rate of the Ar gas flow meter to 55-65 sccm, and use a gas ion source to perform plasma glow discharge cleaning on the substrate under DC bias for 15-20 minutes.

[0016] Preferably, in step S4, the sputtering power of the Al target is 80-150W, the sputtering time of the target is 45-60min, and the substrate temperature during magnetron sputtering is 200-220℃.

[0017] Preferably, in step S5, the power of the Al target is 10-14W, and the power of the AlN target is 100-150W.

[0018] The beneficial effects of this invention are as follows: The titanium alloy substrate, using the above-mentioned technical solution, consists of an Al layer and an AlN-Al layer, arranged sequentially from the inside out. A thin TiO2 oxide film typically forms on the surface of the titanium alloy substrate. This oxide film significantly affects the interfacial strength of the coating, usually greatly reducing the adhesion at the interface. However, according to reaction kinetics, aluminum atoms can spontaneously undergo an in-situ exchange reaction with TiO2, which is an irreversible exothermic reaction (Kinetic evaluation of combustion synthesis 3TiO2+7Al→3TiAl+2Al2O3 using non-isothermal DSC method (Materials Chemistry and Physics, 2005, 91: 140~145)). This reaction produces a large amount of the bonding phase TiAl, which plays a strong connecting role between the coating and the substrate, greatly enhancing the bonding strength between them. Adding a transition layer can effectively reduce the gradient difference in the coefficients of thermal expansion between the coatings, thereby reducing the stress between the substrates. AlN is readily doped with p-type elements (Al, B, Be, Ga, O, etc.), while titanium alloys contain a large amount of Al. Therefore, Al doping is easy to achieve and will not negatively affect the coating's performance. Moreover, adding trace amounts of Al to AlN can significantly reduce the coefficient of friction of the AlN coating and improve its wear resistance. Furthermore, the process of doping Al into AlN coatings is very simple, requiring only an AlN target and an Al target to complete the deposition.

[0019] This invention uses an Al transition layer as an intermediate layer between the coating and the substrate, solving the problem of bonding strength between the two. Al doping in the thin film successfully addresses the high friction coefficient of the AlN coating. Furthermore, since both the intermediate layer material and the dopant are Al, the deposition process and equipment are simplified, allowing the entire deposition process to be completed using a dual-target magnetron sputtering system. The process of this invention yields a smooth surface free of defects such as pores and cracks. This method significantly reduces coating stress and greatly enhances coating adhesion. Attached Figure Description

[0020] Figure 1 This is a scanning electron microscope image of the coating in Example 1.

[0021] Figure 2 This is a scanning electron microscope image of the coating in Comparative Example 1. Implementation

[0022] The present invention will be further described below with reference to specific embodiments: Example

[0023] The method for preparing a coating on the surface of an ultrasonic surgical scalpel by magnetron sputtering mainly includes the following steps:

[0024] S1. Grind, polish, ultrasonically clean, and dry the substrate;

[0025] S2. After wiping the pretreated substrate from step S1 with an alcohol cloth, install it on the sample rotation frame and place it in the magnetron sputtering coating chamber. Select AlN target and Al target as sputtering sources, and ensure that the distance between the substrate surface and the target position is 10cm. The sample rotates inside the sleeve and the rotation frame revolves around the center at a speed of 5r / min.

[0026] S3. After installing the substrate, close the magnetron sputtering coating chamber door and perform plasma glow discharge cleaning on the substrate for 15 minutes. At the same time, start the heater to heat the pre-coated sample.

[0027] S4. Using Al target material as sputtering raw material and Ar gas as sputtering gas, magnetron sputtering was used to prepare the intermediate Al coating layer with a sputtering power of 150W.

[0028] S5. Using Al and AlN targets as sputtering raw materials and Ar gas as sputtering gas, an AlN-Al coating is prepared on the intermediate Al coating by magnetron sputtering. The mass fraction of Al in the AlN-Al coating is 1%. During the sputtering process, the power of the Al target is 10W, the power of the AlN target is 150W, the Ar gas flow rate is 60sccm, the target-substrate distance is 10cm, the sputtering time is 50min, and the substrate temperature is 200℃. Example

[0029] The method for preparing a coating on the surface of an ultrasonic surgical scalpel by magnetron sputtering mainly includes the following steps:

[0030] S1. Grind, polish, ultrasonically clean, and dry the substrate;

[0031] S2. After wiping the pretreated substrate from step S1 with an alcohol cloth, install it on the sample rotation frame and place it in the magnetron sputtering coating chamber. Select AlN target and Al target as sputtering sources, and ensure that the distance between the substrate surface and the target position is 10cm. The sample rotates inside the sleeve and the rotation frame revolves around the center at a speed of 5r / min.

[0032] S3. After installing the substrate, close the magnetron sputtering coating chamber door and perform plasma glow discharge cleaning on the substrate for 15 minutes. At the same time, start the heater to heat the pre-coated sample.

[0033] S4. Using Al target material as sputtering raw material and Ar gas as sputtering gas, magnetron sputtering was used to prepare the intermediate Al coating layer with a sputtering power of 150W.

[0034] S5. Using Al and AlN targets as sputtering raw materials and Ar gas as sputtering gas, an AlN-Al coating is prepared on the intermediate Al coating by magnetron sputtering. The mass fraction of Al in the AlN-Al coating is 1.2%. During the sputtering process, the power of the Al target is 11W, the power of the AlN target is 150W, the Ar gas flow rate is 60sccm, the target-substrate distance is 10cm, the sputtering time is 50min, and the substrate temperature is 200℃. Example

[0035] The method for preparing a coating on the surface of an ultrasonic surgical scalpel by magnetron sputtering mainly includes the following steps:

[0036] S1. Grind, polish, ultrasonically clean, and dry the substrate;

[0037] S2. After wiping the pretreated substrate from step S1 with an alcohol cloth, install it on the sample rotation frame and place it in the magnetron sputtering coating chamber. Select AlN target and Al target as sputtering sources, and ensure that the distance between the substrate surface and the target position is 10cm. The sample rotates inside the sleeve and the rotation frame revolves around the center at a speed of 5r / min.

[0038] S3. After installing the substrate, close the magnetron sputtering coating chamber door and perform plasma glow discharge cleaning on the substrate for 15 minutes. At the same time, start the heater to heat the pre-coated sample.

[0039] S4. Using Al target material as sputtering raw material and Ar gas as sputtering gas, magnetron sputtering was used to prepare the intermediate Al coating layer with a sputtering power of 150W.

[0040] S5. Using Al and AlN targets as sputtering raw materials and Ar gas as sputtering gas, an AlN-Al coating is prepared on the intermediate Al coating by magnetron sputtering. The mass fraction of Al in the AlN-Al coating is 1.4%. During the sputtering process, the power of the Al target is 12W, the power of the AlN target is 150W, the Ar gas flow rate is 60sccm, the target-substrate distance is 10cm, the sputtering time is 50min, and the substrate temperature is 200℃. Example

[0041] The method for preparing a coating on the surface of an ultrasonic surgical scalpel by magnetron sputtering mainly includes the following steps:

[0042] S1. Grind, polish, ultrasonically clean, and dry the substrate;

[0043] S2. After wiping the pretreated substrate from step S1 with an alcohol cloth, install it on the sample rotation frame and place it in the magnetron sputtering coating chamber. Select AlN target and Al target as sputtering sources, ensuring that the distance between the substrate surface and the target position is 9cm. The sample rotates inside the sleeve, and the rotation frame revolves around the center at a speed of 5r / min.

[0044] S3. After installing the substrate, close the magnetron sputtering coating chamber door and perform plasma glow discharge cleaning on the substrate for 15 minutes. At the same time, start the heater to heat the pre-coated sample.

[0045] S4. Using Al target material as sputtering raw material and Ar gas as sputtering gas, magnetron sputtering was used to prepare the intermediate Al coating layer with a sputtering power of 100W.

[0046] S5. Using Al and AlN targets as sputtering raw materials and Ar gas as sputtering gas, an AlN-Al coating is prepared on the intermediate Al coating by magnetron sputtering. The mass fraction of Al in the AlN-Al coating is 1.6%. During the sputtering process, the power of the Al target is 13W, the power of the AlN target is 150W, the Ar gas flow rate is 60sccm, the target-substrate distance is 10cm, the sputtering time is 50min, and the substrate temperature is 200℃. Example

[0047] The method for preparing a coating on the surface of an ultrasonic surgical scalpel by magnetron sputtering mainly includes the following steps:

[0048] S1. Grind, polish, ultrasonically clean, and dry the substrate;

[0049] S2. After wiping the pretreated substrate from step S1 with an alcohol cloth, install it on the sample rotation frame and place it in the magnetron sputtering coating chamber. Select AlN target and Al target as sputtering sources, and ensure that the distance between the substrate surface and the target position is 11cm. The sample rotates inside the sleeve and the rotation frame revolves around the center at a speed of 5r / min.

[0050] S3. After installing the substrate, close the magnetron sputtering coating chamber door and perform plasma glow discharge cleaning for 20 minutes. At the same time, start the heater to heat the pre-coated sample.

[0051] S4. Using Al target material as sputtering raw material and Ar gas as sputtering gas, magnetron sputtering was used to prepare the intermediate Al coating layer with a sputtering power of 80W.

[0052] S5. Using Al and AlN targets as sputtering raw materials and Ar gas as sputtering gas, an AlN-Al coating is prepared on the intermediate Al coating by magnetron sputtering. The mass fraction of Al in the AlN-Al coating is 2.0%. During the sputtering process, the power of the Al target is 14W, the power of the AlN target is 150W, the Ar gas flow rate is 60sccm, the target-substrate distance is 10cm, the sputtering time is 50min, and the substrate temperature is 200℃.

[0053] Comparative Example 1:

[0054] The method for preparing a coating on the surface of an ultrasonic surgical scalpel by magnetron sputtering mainly includes the following steps:

[0055] S1. Grind, polish, ultrasonically clean, and dry the substrate;

[0056] S2. After wiping the substrate pretreated in S1 with an alcohol cloth, the substrate is placed on the sample rotation frame and placed in the magnetron sputtering coating chamber. AlN target and Al target are selected as sputtering sources. The distance between the substrate surface and the target position is 10cm. The sample rotates in the sleeve and the rotation frame revolves around the center at a speed of 5r / min.

[0057] S3. After installing the substrate, close the magnetron sputtering coating chamber door and perform plasma glow discharge cleaning on the substrate for 15 minutes. At the same time, start the heater to heat the pre-coated sample.

[0058] S4. Using Al target material as sputtering raw material and Ar gas as sputtering gas, an intermediate Al coating layer is prepared by magnetron sputtering;

[0059] S5. Using AlN target as sputtering raw material and Ar gas as sputtering gas, an AlN coating was prepared on the intermediate Al coating by magnetron sputtering. The Ar gas flow rate was 60 sccm, the target-substrate distance was 10 cm, the sputtering time was 50 min, and the substrate temperature was 200℃ during the sputtering process.

[0060] Comparative Example 2:

[0061] The method for preparing a coating on the surface of an ultrasonic surgical scalpel by magnetron sputtering mainly includes the following steps:

[0062] S1. Grind, polish, ultrasonically clean, and dry the substrate;

[0063] S2. After wiping the pretreated substrate from step S1 with an alcohol cloth, install it on the sample rotation frame and place it in the magnetron sputtering coating chamber. Select AlN target and Al target as sputtering sources, and ensure that the distance between the substrate surface and the target position is 10cm. The sample rotates inside the sleeve and the rotation frame revolves around the center at a speed of 5r / min.

[0064] S3. After installing the substrate, close the magnetron sputtering coating chamber door and perform plasma glow discharge cleaning on the substrate for 15 minutes. At the same time, start the heater to heat the pre-coated sample.

[0065] S4. Using Al target material as sputtering raw material and Ar gas as sputtering gas, an intermediate Al coating layer is prepared by magnetron sputtering;

[0066] S5. Using Al and AlN targets as sputtering raw materials and Ar gas as sputtering gas, an AlN-Al coating is prepared on the intermediate Al coating by magnetron sputtering. The mass fraction of Al in the AlN-Al coating is 10%. During the sputtering process, the power of the Al target is 50W, the power of the AlN target is 150W, the Ar gas flow rate is 60sccm, the target-substrate distance is 10cm, the sputtering time is 50min, and the substrate temperature is 200℃.

[0067] Further, relevant performance tests were conducted on the coatings of Examples 1-5 and Comparative Examples 1-2.

[0068] Surface morphology observation: The coating surfaces of different examples and comparative examples were observed using a microscope and a scanning electron microscope (SEM).

[0069] Hardness testing: An Agilent Nano Indenter G200 nanoindenter was used for testing. The indenter was made of diamond, and the indentation depth did not exceed 10% of the coating thickness to minimize measurement error. Instrument parameters: Berkovich pyramidal diamond indenter, displacement resolution not exceeding 0.01 nm, load resolution 50 nN, Poisson's ratio λ of 0.32. Each sample was measured 5 times to ensure the reliability and accuracy of the test results.

[0070] Friction resistance test: A UMT-TriboLab reciprocating friction and wear tester manufactured by Bruker GmbH, Germany, was used. The sample was fixed to the sample stage with double-sided tape, ensuring the sample was centered and firmly adhered. The appropriate parameters were set, and the equipment was started to rub the sample in a uniform circular motion. The changes in wear amount and coefficient of friction were compared. The time required for the prepared coating to completely wear off was measured based on the changes in wear amount to determine the friction and wear resistance performance. Friction parameters: The friction pair consisted of 3mm diameter GCr15 steel balls; the load was 5N; the motor speed was 200r / min; the wear radius was 3mm; the test duration was 30min; and the experimental result was the ratio of the coated sample to the Ti-6Al-4V titanium alloy (substrate).

[0071] The test results of Examples 1-5 and Comparative Examples 1-2 are shown in Table 1 below. The scanning electron microscope image of Example 1 is shown below. Figure 1 As shown, the scanning electron microscope image of Comparative Example 1 is as follows: Figure 2 As shown.

[0072] Table 1 Test data for each sample

[0073] Surface morphology Hardness / GPa Abrasion resistance / times Example 1 Smooth, dense and crack-free 7.43 2.1 Example 2 Smooth, dense and crack-free 8.03 2.4 Example 3 Smooth, dense and crack-free 7.14 1.9 Example 4 Smooth, dense and crack-free 6.91 1.8 Example 5 Smooth, dense and crack-free 6.76 1.7 Comparative Example 1 Rough surface with cracks 3.62 1 Comparative Example 2 Smooth, dense and crack-free 5.61 1.5

[0074] By comparing the examples and comparative examples, it can be seen that adding a transition layer Al coating to the titanium alloy substrate and AlN coating, and doping with Al element to form a novel composite coating material, can significantly improve the surface smoothness and density. In addition, it also improves the hardness and wear resistance of the coating.

Claims

1. A method for preparing a coating on the surface of an ultrasonic surgical scalpel by magnetron sputtering, wherein the substrate of the ultrasonic surgical scalpel is made of titanium alloy, characterized in that... Specifically, the following steps are included: S1. Pre-treatment of the substrate surface: grinding, polishing, ultrasonic cleaning, and drying the substrate; S2. Loading: The pretreated substrate from step S1 is mounted on the sample rotating frame and placed into the magnetron sputtering coating chamber; S3. Glow Glow Cleaning: Perform plasma glow cleaning on the substrate for 15-20 minutes, while simultaneously starting the heater to heat the pre-coated sample. S4. Preparation of intermediate coating: Using Al target as sputtering raw material and Ar gas as sputtering gas, the intermediate Al coating is prepared by magnetron sputtering. S5. Coating preparation: Using Al and AlN targets as sputtering raw materials and Ar gas as sputtering gas, an AlN-Al coating is prepared on the intermediate Al coating by magnetron sputtering. The mass fraction of Al in the AlN-Al coating is 1%-2%.

2. The method of claim 1, wherein the coating is prepared by surface magnetron sputtering. The matrix material is Ti-6Al-4V titanium alloy.

3. The method of claim 1, wherein the coating is prepared by surface magnetron sputtering. In step S1, the substrate is successively polished with 400-grit, 800-grit, 1500-grit, and 2000-grit sandpaper, then polished on a polishing machine, then cleaned with acetone degreasing agent for 40 minutes, ultrasonically cleaned with pure water for 40 minutes, and finally dried with an air gun.

4. The method of claim 1, wherein the coating is prepared by surface magnetron sputtering. In step S2, the distance between the substrate surface and the target position is 9-11 cm.

5. The method of claim 1, wherein the coating is prepared by surface magnetron sputtering. Step S3 includes: evacuating to a vacuum level of 1×10⁻⁶. -3 Pa, open the Ar gas cylinder to fill the vacuum membrane cavity with Ar gas, adjust the flow rate of the Ar gas flow meter to 55-65 sccm, and use a gas ion source to perform plasma glow discharge cleaning on the substrate under DC bias for 15-20 minutes.

6. The method for preparing a coating on the surface of an ultrasonic surgical scalpel by magnetron sputtering according to claim 1, characterized in that, In step S4, the sputtering power of the Al target is 80-150W, the sputtering time of the target is 45-60min, and the substrate temperature during magnetron sputtering is 200-220℃.

7. The method of claim 1, wherein the coating is prepared by surface magnetron sputtering. In step S5, the power of the Al target is 10-14W, and the power of the AlN target is 100-150W.

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