A surgical instrument and its preparation method

Abstract

This invention relates to the field of magnetron sputtering coatings, specifically disclosing a surgical instrument and its preparation method. This invention utilizes cold isostatic pressing (CIP) to treat a TiNO coating. Studies have shown that CIP treatment is beneficial for improving the corrosion resistance of TiNO coatings on stainless steel substrates; however, the reduction in self-corrosion current density gradually weakens with increasing treatment time. Regarding the hardness of the coating material, the hardness initially increases and then decreases with increasing CIP treatment time. Therefore, in practical applications, the CIP treatment time needs to be strictly controlled.

Description

Technical Field

[0001] This invention relates to the field of magnetron sputtering coatings, and more specifically to a surgical instrument and its preparation method. Background Technology

[0002] Surgical instruments are indispensable medical devices in surgical procedures. A scalpel typically consists of a blade and a handle, and is a specially designed tool for cutting human or animal tissue. Surgical blades are usually made of pure titanium, titanium alloys, stainless steel, or carbon steel. These materials require excellent cutting performance and corrosion resistance to meet the cutting demands of surgical procedures.

[0003] Chinese patent CN202111087093.2 describes the preparation of a TiNO tool coating using magnetron sputtering, which exhibits satisfactory hydrophilicity angle, hardness, hemolysis rate, and tissue adhesion. However, the corrosion resistance of this surgical tool is poor, directly impacting its service life. Summary of the Invention

[0004] The purpose of this invention is to provide a method for preparing surgical instruments, wherein the surgical instrument material prepared by this method has excellent hardness and corrosion resistance.

[0005] The technical solution of the present invention is as follows:

[0006] A method for preparing a surgical instrument includes the following steps:

[0007] Substrate pretreatment: Stainless steel is used as the substrate material for surgical instruments. It is successively ground, polished, acid-washed, degreased, cleaned and dried for use. The acid washing uses 10-20% HF solution, the degreasing uses 20-25% NaOH solution, and then anhydrous ethanol and deionized water are used for cleaning, and then dried under inert gas.

[0008] Preparation of TiNO coating: A dried stainless steel substrate was placed in a magnetron sputtering coating machine, and a TiNO coating was prepared in a mixed atmosphere of oxygen and nitrogen using titanium as the sputtering source. The base vacuum was 5 × 10⁻⁶. -2 Pa, sputtering temperature is 200-220℃, substrate bias voltage is -200~-220V, target current is 25-30A, sputtering time is 45-60min, total gas flow rate is 100-120sccm, and oxygen to nitrogen flow ratio is 1∶3-5.

[0009] Cold isostatic pressing: Place the stainless steel substrate with TiNO coating into a cold isostatic press and perform cold isostatic pressing for 30-150 minutes under a pressure of 90-100MPa.

[0010] Vacuum annealing: The tool material after cold isostatic pressing is placed in a vacuum annealing furnace and annealed for 3-5 hours at a temperature of 550-600℃.

[0011] Preferably, the annealing time is 3 hours.

[0012] Preferably, the annealing temperature is 600°C.

[0013] Preferably, the pressure of the cold isostatic pressing is 90 MPa.

[0014] Preferably, the cold isostatic pressing treatment time is 57 minutes.

[0015] Preferably, the flow rate ratio of oxygen to nitrogen is 1:3.

[0016] Furthermore, the present invention also provides a surgical instrument prepared by the above method.

[0017] This invention utilizes cold isostatic pressing (CIP) to treat TiNO coatings. Studies have shown that CIP treatment improves the corrosion resistance of TiNO coatings on stainless steel substrates; however, the reduction in self-corrosion current density gradually weakens with increasing treatment time. Regarding the hardness of the coating material, the hardness initially increases and then decreases with increasing CIP treatment time. Therefore, in practical applications, the CIP treatment time needs to be strictly controlled. Detailed Implementation

[0018] The technical effects of the present invention will be verified through specific embodiments below, but the implementation of the present invention is not limited thereto.

[0019] Example 1

[0020] Substrate pretreatment: Stainless steel is used as the substrate material. It is successively ground, polished, pickled, degreased, cleaned and dried for later use. The pickling is done with 10% HF solution and the degreasing is done with 20% NaOH solution. Then, anhydrous ethanol and deionized water are used for cleaning and drying under inert gas.

[0021] Preparation of TiNO coating: A dried stainless steel substrate was placed in a magnetron sputtering coating machine, and a TiNO coating was prepared in a mixed atmosphere of oxygen and nitrogen using titanium as the sputtering source. The base vacuum was 5 × 10⁻⁶. -2 Pa, sputtering temperature is 200℃, substrate bias voltage is -200V, target current is 30A, sputtering time is 45min, total gas flow rate is 100sccm, and oxygen to nitrogen flow ratio is 1:3.

[0022] Cold isostatic pressing: The stainless steel substrate with TiNO coating is placed in a cold isostatic press and cold isostatically pressed for 30 minutes at a pressure of 90 MPa.

[0023] Vacuum annealing: The tool material after cold isostatic pressing is placed in a vacuum annealing furnace and annealed for 3 hours at a temperature of 600℃.

[0024] Example 2

[0025] Substrate pretreatment: Stainless steel is used as the substrate material. It is successively ground, polished, pickled, degreased, cleaned and dried for later use. The pickling is done with 10% HF solution and the degreasing is done with 20% NaOH solution. Then, anhydrous ethanol and deionized water are used for cleaning and drying under inert gas.

[0026] Preparation of TiNO coating: A dried stainless steel substrate was placed in a magnetron sputtering coating machine, and a TiNO coating was prepared in a mixed atmosphere of oxygen and nitrogen using titanium as the sputtering source. The base vacuum was 5 × 10⁻⁶. -2 Pa, sputtering temperature is 200℃, substrate bias voltage is -200V, target current is 30A, sputtering time is 45min, total gas flow rate is 100sccm, and oxygen to nitrogen flow ratio is 1:3.

[0027] Cold isostatic pressing: The stainless steel substrate with TiNO coating is placed in a cold isostatic press and cold isostatically pressed for 57 minutes at a pressure of 90 MPa.

[0028] Vacuum annealing: The tool material after cold isostatic pressing is placed in a vacuum annealing furnace and annealed for 3 hours at a temperature of 600℃.

[0029] Example 3

[0030] Substrate pretreatment: Stainless steel is used as the substrate material. It is successively ground, polished, pickled, degreased, cleaned and dried for later use. The pickling is done with 10% HF solution and the degreasing is done with 20% NaOH solution. Then, anhydrous ethanol and deionized water are used for cleaning and drying under inert gas.

[0031] Preparation of TiNO coating: A dried stainless steel substrate was placed in a magnetron sputtering coating machine, and a TiNO coating was prepared in a mixed atmosphere of oxygen and nitrogen using titanium as the sputtering source. The base vacuum was 5 × 10⁻⁶. -2 Pa, sputtering temperature is 200℃, substrate bias voltage is -200V, target current is 30A, sputtering time is 45min, total gas flow rate is 100sccm, and oxygen to nitrogen flow ratio is 1:3.

[0032] Cold isostatic pressing: The stainless steel substrate with TiNO coating is placed in a cold isostatic press and cold isostatically pressed for 90 min at a pressure of 90 MPa.

[0033] Vacuum annealing: The tool material after cold isostatic pressing is placed in a vacuum annealing furnace and annealed for 3 hours at a temperature of 600℃.

[0034] Example 4

[0035] Substrate pretreatment: Stainless steel is used as the substrate material. It is successively ground, polished, pickled, degreased, cleaned and dried for later use. The pickling is done with 10% HF solution and the degreasing is done with 20% NaOH solution. Then, anhydrous ethanol and deionized water are used for cleaning and drying under inert gas.

[0036] Preparation of TiNO coating: A dried stainless steel substrate was placed in a magnetron sputtering coating machine, and a TiNO coating was prepared in a mixed atmosphere of oxygen and nitrogen using titanium as the sputtering source. The base vacuum was 5 × 10⁻⁶. -2 Pa, sputtering temperature is 200℃, substrate bias voltage is -200V, target current is 30A, sputtering time is 45min, total gas flow rate is 100sccm, and oxygen to nitrogen flow ratio is 1:3.

[0037] Cold isostatic pressing: The stainless steel substrate with TiNO coating is placed in a cold isostatic press and cold isostatically pressed for 120 minutes at a pressure of 90 MPa.

[0038] Vacuum annealing: The tool material after cold isostatic pressing is placed in a vacuum annealing furnace and annealed for 3 hours at a temperature of 600℃.

[0039] Example 5

[0040] Substrate pretreatment: Stainless steel is used as the substrate material. It is successively ground, polished, pickled, degreased, cleaned and dried for later use. The pickling is done with 10% HF solution and the degreasing is done with 20% NaOH solution. Then, anhydrous ethanol and deionized water are used for cleaning and drying under inert gas.

[0041] Preparation of TiNO coating: A dried stainless steel substrate was placed in a magnetron sputtering coating machine, and a TiNO coating was prepared in a mixed atmosphere of oxygen and nitrogen using titanium as the sputtering source. The base vacuum was 5 × 10⁻⁶. -2 Pa, sputtering temperature is 200℃, substrate bias voltage is -200V, target current is 30A, sputtering time is 45min, total gas flow rate is 100sccm, and oxygen to nitrogen flow ratio is 1:3.

[0042] Cold isostatic pressing: The stainless steel substrate with TiNO coating is placed in a cold isostatic press and cold isostatically pressed for 150 min at a pressure of 90 MPa.

[0043] Vacuum annealing: The tool material after cold isostatic pressing is placed in a vacuum annealing furnace and annealed for 3 hours at a temperature of 600℃.

[0044] Comparative Example 1

[0045] Substrate pretreatment: Stainless steel is used as the substrate material. It is successively ground, polished, pickled, degreased, cleaned and dried for later use. The pickling is done with 10% HF solution and the degreasing is done with 20% NaOH solution. Then, anhydrous ethanol and deionized water are used for cleaning and drying under inert gas.

[0046] Preparation of TiNO coating: A dried stainless steel substrate was placed in a magnetron sputtering coating machine, and a TiNO coating was prepared in a mixed atmosphere of oxygen and nitrogen using titanium as the sputtering source. The base vacuum was 5 × 10⁻⁶. -2 Pa, sputtering temperature is 200℃, substrate bias voltage is -200V, target current is 30A, sputtering time is 45min, total gas flow rate is 100sccm, and oxygen to nitrogen flow ratio is 1:3.

[0047] Vacuum annealing: The stainless steel substrate with TiNO coating is placed in a vacuum annealing furnace and annealed for 3 hours at a temperature of 600℃.

[0048] Comparative Example 2

[0049] Substrate pretreatment: Stainless steel is used as the substrate material. It is successively ground, polished, pickled, degreased, cleaned and dried for later use. The pickling is done with 10% HF solution and the degreasing is done with 20% NaOH solution. Then, anhydrous ethanol and deionized water are used for cleaning and drying under inert gas.

[0050] Preparation of TiNO coating: A dried stainless steel substrate was placed in a magnetron sputtering coating machine, and a TiNO coating was prepared in a mixed atmosphere of oxygen and nitrogen using titanium as the sputtering source. The base vacuum was 5 × 10⁻⁶. -2 Pa, sputtering temperature is 200℃, substrate bias voltage is -200V, target current is 30A, sputtering time is 45min, total gas flow rate is 100sccm, and oxygen to nitrogen flow ratio is 1:3.

[0051] Cold isostatic pressing: The stainless steel substrate with TiNO coating is placed in a cold isostatic press and cold isostatically pressed for 300 min at a pressure of 90 MPa.

[0052] Vacuum annealing: The tool material after cold isostatic pressing is placed in a vacuum annealing furnace and annealed for 3 hours at a temperature of 600℃.

[0053] The hardness and corrosion resistance of the experimental samples in Examples 1-5 and Comparative Examples 1-2 were evaluated using the following methods:

[0054] Hardness test: Nano-indenter G200 nano-indenter was used to perform nano-indentation experiments on the coating material to obtain the hardness data of the coating material. Berkovich triangular pyramidal diamond indenter was used in the experiment, and the indentation depth did not exceed 10% of the coating thickness.

[0055] Corrosion resistance: Electrochemical tests were conducted on each sample using an electrochemical workstation in an 8.5 wt% NaCl medium solution. Non-working surfaces were sealed with nail polish, and the exposed working surface area was 2.5 cm². 2 The test was conducted at room temperature.

[0056] The experimental results are shown in Table 1.

[0057] Table 1 Experimental data for each sample

[0058]

[0059] As shown in Table 1, cold isostatic pressing (COP) is beneficial for improving the corrosion resistance of the TiNO coating on the stainless steel substrate. However, the reduction in self-corrosion current density gradually weakens with increasing processing time. Regarding the hardness of the coating material, the hardness first increases and then decreases with increasing COP time. Therefore, in practical applications, the COP time needs to be strictly controlled. Considering both the hardness and corrosion resistance of the tool coating material, Example 2 is the most preferred technical solution.

[0060] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the technical principles of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A surgical instrument, characterized in that, The preparation process of the surgical instrument includes the following steps: Substrate pretreatment: Stainless steel is used as the substrate material for surgical instruments. It is successively ground, polished, acid-washed, degreased, cleaned and dried for use. The acid washing uses 10-20% HF solution, the degreasing uses 20-25% NaOH solution, and then anhydrous ethanol and deionized water are used for cleaning, and then dried under inert gas. Preparation of TiNO coating: A dried stainless steel substrate was placed in a magnetron sputtering coating machine, and a TiNO coating was prepared in a mixed atmosphere of oxygen and nitrogen using titanium as the sputtering source. The base vacuum was 5 × 10⁻⁶. -2 Pa, sputtering temperature is 200-220℃, substrate bias voltage is -200~-220V, target current is 25-30A, sputtering time is 45-60min, total gas flow rate is 100-120sccm, and oxygen to nitrogen flow ratio is 1∶3-5. Cold isostatic pressing: Place the stainless steel substrate with TiNO coating into a cold isostatic press and cold isostatic press for 57-90 min at a pressure of 90-100 MPa. Vacuum annealing: The tool material after cold isostatic pressing is placed in a vacuum annealing furnace and annealed for 3-5 hours at a temperature of 550-600℃.

2. The surgical instrument as described in claim 1, characterized in that, The annealing time is 3 hours.

3. The surgical instrument as described in claim 1, characterized in that, The annealing temperature is 600℃.

4. The surgical instrument as described in claim 1, characterized in that, The pressure for the cold isostatic pressing process is 90 MPa.

5. The surgical instrument as described in claim 1, characterized in that, The cold isostatic pressing process takes 57 minutes.

6. The surgical instrument as described in claim 1, characterized in that, The flow rate ratio of oxygen to nitrogen is 1:3.

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