Surface coating material for thyroid retractor and preparation method thereof

Abstract

A surface coating material for a thyroid retractor and a preparation method thereof. In order to improve the corrosion resistance of a stainless steel thyroid retractor, the present invention prepares a DLC-HfO2 composite coating on the surface of a stainless steel substrate. Studies have shown that with the increase of the HfO2 content, the corrosion resistance of the DLC-HfO2 composite coating shows a trend of first increasing and then stabilizing. However, when the HfO2 content is too high, the higher hemolysis rate determines that it is not suitable as a medical material. Therefore, in actual use, the HfO2 content in the composite coating should be controlled at 5.2wt%-19wt%.

Description

Technical Field

[0001] The present invention relates to the field of magnetron sputtering coatings (C23C14 / 35), and in particular to a surface coating material for a thyroid retractor and a preparation method thereof. Background Art

[0002] A thyroid retractor is a tool used to pull adjacent tissues during thyroid surgery, facilitating smoother thyroid surgery. It's primarily used to expose the thyroid gland and surrounding tissues during thyroid surgery, allowing the surgeon to more clearly visualize the surgical area and perform precise procedures. It retracts the skin, subcutaneous tissue, muscle, and fascia, providing a clear, unobstructed field of view and facilitating delicate surgical procedures.

[0003] The corrosion resistance of the stainless steel thyroid retractor in the prior art is not ideal, which seriously affects its service life. In view of this, it is urgent to design a thyroid retractor with excellent corrosion resistance. Summary of the Invention

[0004] The object of the present invention is to provide a method for preparing a surface coating material for a thyroid retractor, wherein the surface coating material for a thyroid retractor prepared by the method has excellent corrosion resistance.

[0005] The technical solutions of the present invention are as follows:

[0006] A method for preparing a surface coating material for a thyroid retractor, comprising the following steps:

[0007] Liner pretreatment: Use stainless steel as the substrate material, use sandpaper to polish the substrate to remove surface burrs, then use 10-15% hydrochloric acid solution to pickle for 30-60 minutes to remove surface oxides, use 15-20% OP-10 emulsifier to clean for 15-20 minutes to remove surface grease, then rinse in deionized water for 30-60 minutes, and finally dry under nitrogen for use.

[0008] Preparation of DLC-HfO2 composite coating: The stainless steel substrate was placed in a magnetron sputtering coating device, and a graphite target and an HfO2 target were used as sputtering sources. A DLC-HfO2 composite coating with a thickness of 8-10 nm was formed by co-sputtering under argon conditions. During the sputtering process, the background vacuum was 1.0×10 -2 Pa, sputtering temperature is 160-180℃, substrate bias voltage is -220~-200V, argon flow rate is 60-80sccm, and the HfO2 content in the composite coating is 5.2-19.0wt% by adjusting the sputtering power of the two targets;

[0009] Stress relief annealing: Place the substrate material containing the DLC-HfO2 composite coating in an annealing furnace and anneal for 2.5-2.8 hours at an annealing temperature of 420-450°C.

[0010] Preferably, the concentration of the hydrochloric acid solution is 15%.

[0011] Preferably, the thickness is 8 nm.

[0012] Preferably, the sputtering temperature is 180°C.

[0013] Preferably, the gas flow rate is 80 sccm.

[0014] Preferably, the content of HfO2 in the composite coating is 15.3 wt%.

[0015] Furthermore, the present invention also provides a surface coating material for a thyroid retractor, and the coating material is prepared by the above method.

[0016] To improve the corrosion resistance of stainless steel thyroid retractors, the present invention fabricated a DLC-HfO2 composite coating on the surface of a stainless steel substrate. Studies have shown that the corrosion resistance of the DLC-HfO2 composite coating increases with increasing HfO2 content, initially increasing and then stabilizing. However, when the HfO2 content is too high, the high hemolysis rate makes it unsuitable for medical use. Therefore, in practical applications, the HfO2 content of the composite coating should be controlled between 5.2wt% and 19wt%. DETAILED DESCRIPTION

[0017] The technical effects of the present invention are verified below through specific examples, but the embodiments of the present invention are not limited thereto.

[0018] Example 1

[0019] Substrate pretreatment: Stainless steel was used as the substrate material. Sandpaper was used to polish the substrate to remove burrs on the surface. Then, 15% hydrochloric acid solution was used for pickling for 30 minutes to remove surface oxides. 20% OP-10 emulsifier was used for cleaning for 15 minutes to remove surface grease. The substrate was then rinsed in deionized water for 30 minutes and dried under nitrogen for later use.

[0020] Preparation of DLC-HfO2 composite coating: The stainless steel substrate was placed in a magnetron sputtering coating device, and a graphite target and an HfO2 target were used as sputtering sources. A DLC-HfO2 composite coating with a thickness of 8 nm was formed by co-sputtering under argon conditions. During the sputtering process, the background vacuum was 1.0×10 -2Pa, the sputtering temperature was 180 °C, the substrate bias was -220 V, the argon flow rate was 80 sccm, and the HfO2 content in the composite coating was 5.2 wt% by adjusting the sputtering power of the two targets;

[0021] Stress relief annealing: The substrate material containing the DLC-HfO2 composite coating is placed in an annealing furnace and annealed for 2.5 hours at an annealing temperature of 420°C.

[0022] Example 2

[0023] Substrate pretreatment: Stainless steel was used as the substrate material. Sandpaper was used to polish the substrate to remove burrs on the surface. Then, 15% hydrochloric acid solution was used for pickling for 30 minutes to remove surface oxides. 20% OP-10 emulsifier was used for cleaning for 15 minutes to remove surface grease. The substrate was then rinsed in deionized water for 30 minutes and dried under nitrogen for later use.

[0024] Preparation of DLC-HfO2 composite coating: The stainless steel substrate was placed in a magnetron sputtering coating device, and a graphite target and an HfO2 target were used as sputtering sources. A DLC-HfO2 composite coating with a thickness of 8 nm was formed by co-sputtering under argon conditions. During the sputtering process, the background vacuum was 1.0×10 -2 Pa, the sputtering temperature was 180 °C, the substrate bias was -220 V, the argon flow rate was 80 sccm, and the HfO2 content in the composite coating was 8.0 wt% by adjusting the sputtering power of the two targets;

[0025] Stress relief annealing: The substrate material containing the DLC-HfO2 composite coating is placed in an annealing furnace and annealed for 2.5 hours at an annealing temperature of 420°C.

[0026] Example 3

[0027] Substrate pretreatment: Stainless steel was used as the substrate material. Sandpaper was used to polish the substrate to remove burrs on the surface. Then, 15% hydrochloric acid solution was used for pickling for 30 minutes to remove surface oxides. 20% OP-10 emulsifier was used for cleaning for 15 minutes to remove surface grease. The substrate was then rinsed in deionized water for 30 minutes and dried under nitrogen for later use.

[0028] Preparation of DLC-HfO2 composite coating: The stainless steel substrate was placed in a magnetron sputtering coating device, and a graphite target and an HfO2 target were used as sputtering sources. A DLC-HfO2 composite coating with a thickness of 8 nm was formed by co-sputtering under argon conditions. During the sputtering process, the background vacuum was 1.0×10 -2 Pa, the sputtering temperature was 180 °C, the substrate bias was -220 V, the argon flow rate was 80 sccm, and the HfO2 content in the composite coating was 12 wt% by adjusting the sputtering power of the two targets;

[0029] Stress relief annealing: The substrate material containing the DLC-HfO2 composite coating is placed in an annealing furnace and annealed for 2.5 hours at an annealing temperature of 420°C.

[0030] Example 4

[0031] Substrate pretreatment: Stainless steel was used as the substrate material. Sandpaper was used to polish the substrate to remove burrs on the surface. Then, 15% hydrochloric acid solution was used for pickling for 30 minutes to remove surface oxides. 20% OP-10 emulsifier was used for cleaning for 15 minutes to remove surface grease. The substrate was then rinsed in deionized water for 30 minutes and dried under nitrogen for later use.

[0032] Preparation of DLC-HfO2 composite coating: The stainless steel substrate was placed in a magnetron sputtering coating device, and a graphite target and an HfO2 target were used as sputtering sources. A DLC-HfO2 composite coating with a thickness of 8 nm was formed by co-sputtering under argon conditions. During the sputtering process, the background vacuum was 1.0×10 -2 Pa, the sputtering temperature was 180 °C, the substrate bias was -220 V, the argon flow rate was 80 sccm, and the HfO2 content in the composite coating was 15.3 wt% by adjusting the sputtering power of the two targets;

[0033] Stress relief annealing: The substrate material containing the DLC-HfO2 composite coating is placed in an annealing furnace and annealed for 2.5 hours at an annealing temperature of 420°C.

[0034] Example 5

[0035] Substrate pretreatment: Stainless steel was used as the substrate material. Sandpaper was used to polish the substrate to remove burrs on the surface. Then, 15% hydrochloric acid solution was used for pickling for 30 minutes to remove surface oxides. 20% OP-10 emulsifier was used for cleaning for 15 minutes to remove surface grease. The substrate was then rinsed in deionized water for 30 minutes and dried under nitrogen for later use.

[0036] Preparation of DLC-HfO2 composite coating: The stainless steel substrate was placed in a magnetron sputtering coating device, and a graphite target and an HfO2 target were used as sputtering sources. A DLC-HfO2 composite coating with a thickness of 8 nm was formed by co-sputtering under argon conditions. During the sputtering process, the background vacuum was 1.0×10 -2 Pa, the sputtering temperature was 180 °C, the substrate bias was -220 V, the argon flow rate was 80 sccm, and the HfO2 content in the composite coating was 19.0 wt% by adjusting the sputtering power of the two targets;

[0037] Stress relief annealing: The substrate material containing the DLC-HfO2 composite coating is placed in an annealing furnace and annealed for 2.5 hours at an annealing temperature of 420°C.

[0038] Comparative Example 1

[0039] Substrate pretreatment: Stainless steel was used as the substrate material. Sandpaper was used to polish the substrate to remove burrs on the surface. Then, 15% hydrochloric acid solution was used for pickling for 30 minutes to remove surface oxides. 20% OP-10 emulsifier was used for cleaning for 15 minutes to remove surface grease. The substrate was then rinsed in deionized water for 30 minutes and dried under nitrogen for later use.

[0040] Preparation of DLC coating: The stainless steel substrate was placed in a magnetron sputtering coating device, and a graphite target was used as the sputtering source. A DLC coating with a thickness of 8 nm was formed under argon conditions. During the sputtering process, the background vacuum was 1.0×10 -2 Pa, sputtering temperature was 180 °C, substrate bias voltage was −220 V, and argon flow rate was 80 sccm;

[0041] Stress relief annealing: The substrate material including the DLC coating is placed in an annealing furnace and annealed for 2.5 hours at an annealing temperature of 420°C.

[0042] Comparative Example 2

[0043] Substrate pretreatment: Stainless steel was used as the substrate material. Sandpaper was used to polish the substrate to remove burrs on the surface. Then, 15% hydrochloric acid solution was used for pickling for 30 minutes to remove surface oxides. 20% OP-10 emulsifier was used for cleaning for 15 minutes to remove surface grease. The substrate was then rinsed in deionized water for 30 minutes and dried under nitrogen for later use.

[0044] Preparation of DLC-HfO2 composite coating: The stainless steel substrate was placed in a magnetron sputtering coating device, and a graphite target and an HfO2 target were used as sputtering sources. A DLC-HfO2 composite coating with a thickness of 8 nm was formed by co-sputtering under argon conditions. During the sputtering process, the background vacuum was 1.0×10 -2 Pa, the sputtering temperature was 180 °C, the substrate bias was -220 V, the argon flow rate was 80 sccm, and the HfO2 content in the composite coating was 30 wt% by adjusting the sputtering power of the two targets;

[0045] Stress relief annealing: The substrate material containing the DLC-HfO2 composite coating is placed in an annealing furnace and annealed for 2.5 hours at an annealing temperature of 420°C.

[0046] Next, the corrosion resistance of the experimental samples in Examples 1-5 and Comparative Examples 1-2 was evaluated. The specific method was as follows: an electrochemical test was performed on each sample in an 8.5 wt% NaCl medium solution using an electrochemical workstation. The non-working surface was sealed with nail polish, and the exposed area of ​​the working surface was 2.5 cm 2, the test was carried out at room temperature. The experimental results are shown in Table 1.

[0047] Table 1 Self-corrosion current density of each sample

[0048] serial number <![CDATA[Self-corrosion current density A / cm 2 > Example 1 <![CDATA[1.03×10 -6 ]]> Example 2 <![CDATA[8.37×10 -7 ]]> Example 3 <![CDATA[5.19×10 -7 ]]> Example 4 <![CDATA[2.10×10 -7 ]]> Example 5 <![CDATA[2.51×10 -7 ]]> Comparative Example 1 <![CDATA[5.11×10 -6 ]]> Comparative Example 2 <![CDATA[2.44×10 -7 ]]>

[0049] As can be seen from Table 1, the DLC-HfO2 composite coating prepared by the present invention can significantly improve the corrosion resistance of stainless steel materials. Moreover, as the HfO2 content increases, the corrosion resistance of the composite coating shows a trend of first increasing and then stabilizing. However, when we conducted a hemolysis test on the test sample in Comparative Example 2, we found that its hemolysis rate was as high as 12.4% (not suitable for use as a medical material), while the hemolysis rates of the samples in Examples 1-5 were all less than 5%. Therefore, in actual use, the HfO2 content in the composite coating should be controlled at 5.2wt%-19wt%.

[0050] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the technical principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing a surface coating material for a thyroid retractor, characterized in that: The following steps are involved: Substrate pretreatment: Use stainless steel as the substrate material, polish the substrate with sandpaper to remove surface burrs, then use 10-15% hydrochloric acid solution to pickle for 30-60 minutes to remove surface oxides, use 15-20% OP-10 emulsifier to clean for 15-20 minutes to remove surface grease, then rinse in deionized water for 30-60 minutes, and finally dry under nitrogen for use. Preparation of DLC-HfO2 composite coating: The stainless steel substrate was placed in a magnetron sputtering coating device, and a graphite target and an HfO2 target were used as sputtering sources. A DLC-HfO2 composite coating with a thickness of 8-10 nm was formed by co-sputtering under argon conditions. During the sputtering process, the background vacuum was 1.0×10 -2 Pa, sputtering temperature of 160-180℃, substrate bias of -220~-200V, argon flow rate of 60-80sccm, by adjusting the sputtering power of the two targets, the HfO2 content in the composite coating was 8.0-19.0wt%; Stress relief annealing: Place the substrate material containing the DLC-HfO2 composite coating in an annealing furnace and anneal for 2.5-2.8 hours at an annealing temperature of 420-450°C.

2. A preparation method according to claim 1, characterized in that: The concentration of the hydrochloric acid solution is 15%.

3. A preparation method according to claim 1, characterized in that: The thickness is 8 nm.

4. A preparation method according to claim 1, characterized in that: The sputtering temperature is 180°C.

5. A preparation method according to claim 1, characterized in that: The gas flow rate is 80 sccm.

6. A preparation method according to claim 1, characterized in that: The content of HfO2 in the composite coating is 15.3 wt%.

7. A surface coating material for a thyroid retractor, characterized in that: The coating material is prepared by the method according to any one of claims 1 to 6.