A low-temperature anti-stick coating for high-frequency electric knife and preparation method thereof

Abstract

The present invention discloses a low-temperature anti-stick coating for a high-frequency electric knife and a preparation method thereof, and relates to the field of surface modification technology. The preparation method of the low-temperature anti-stick coating for a high-frequency electric knife of the present invention comprises at least the following preparation steps: surface treatment and electrochemical polishing of the high-frequency electric knife substrate; mechanical stirring of hydrophobic modified ceramic powder, fusible polytetrafluoroethylene powder and silicone oil modified carbon nanotubes to obtain a mixed powder; baking the mixed powder at 50-60°C for 2-3h, and then spraying the mixed powder on the surface of the electrochemically polished high-frequency electric knife substrate through an atmospheric plasma spraying process to obtain a low-temperature anti-stick coating. The low-temperature anti-stick coating for a high-frequency electric knife prepared by the present invention has a strong bonding force with the base material, and has the properties of anti-blood adhesion, anti-tissue adhesion, and low-temperature storage resistance.

Description

Technical Field

[0001] The invention relates to the technical field of surface modification, and in particular to a low-temperature anti-stick coating for a high-frequency electric knife and a preparation method thereof. Background Art

[0002] While treating patients' diseases, modern medicine pays more attention to the improvement and rehabilitation of patients' psychological and physiological pain, quality of life, and is considerate to patients to the greatest extent and relieves their pain. Compared with traditional surgery, minimally invasive surgery has the advantages of reducing pain, reducing the area of ​​trauma and accelerating postoperative recovery, greatly reducing the inconvenience and pain brought to patients by the disease. The invention of electrosurgical instruments has laid a solid foundation for the realization of minimally invasive surgery, realizing the synchronization of tissue cutting and hemostasis, effectively reducing the amount of blood loss of patients, reducing surgical costs and postoperative risks, and improving surgical efficiency and success rate. The invention and application of high-frequency electric knives have made great contributions. High-frequency electric knives use high-frequency and high-voltage currents to flow through human tissues, causing the charged particles in the cells to oscillate violently and rub against each other, generating a large amount of heat, inducing cell explosion and vaporization, and tissue protein denaturation and coagulation, so as to achieve the purpose of cutting and hemostasis.

[0003] The heat generated by the high-frequency electrosurgical knife is limited to the local tissue in the electrode action area. It has a good coagulation effect, which can reduce the patient's blood loss and blood transfusion volume, and can sterilize the wound during the operation, thereby improving the efficiency and success rate of the operation. However, when the high-frequency electrosurgical knife is used for a long time, the operating temperature of the electrosurgical knife is relatively high, and the blood and soft tissue attached to the surface are prone to dehydration and scab, causing blood and tissue to adhere to the surface and form eschar, thereby reducing the electrical conductivity and thermal conductivity, affecting the field of vision and surgical effect. Tissue adhesion on the surface of the electrosurgical knife may also cause the patient's tissue to tear, making the wound difficult to heal and increasing the patient's pain. Therefore, how to solve the problem of tissue adhesion during the use of high-frequency electrosurgical knife is an urgent problem to be solved.

[0004] At present, the anti-adhesion measures on the surface of high-frequency electrosurgical knives can be mainly divided into the following three types: changing the structure of the electrosurgical knives, changing the microstructure of the surface of the electrosurgical knives, and covering the surface of the electrosurgical knives with a coating. Among them, the improved methods of changing the structure of the electrosurgical knives and changing the microstructure of the surface of the electrosurgical knives have a complex processing process, which is difficult to achieve large-scale production, and the anti-adhesion effect is also relatively limited. In comparison, the method of covering the surface of the electrosurgical knives with a coating does not require changing the original shape of the electrosurgical knives, has a lower processing difficulty, and is more feasible in large-scale production. However, among the coatings currently applied, the strength of the alloy coating is low and easy to peel off, and the polymer coating is easy to decompose at high temperatures and maintains anti-adhesion performance for a long time in a low-temperature environment. In addition, most of the existing coatings have poor conductivity and cannot be applied to the surface of electrosurgical knives. Therefore, it is crucial to prepare a coating with high membrane-based bonding strength, good conductivity, and strong anti-adhesion on the surface of high-frequency electrosurgical knives. Summary of the invention

[0005] The purpose of the present invention is to provide a low-temperature anti-stick coating for high-frequency electric knife and a preparation method thereof, so as to solve the following technical problems: The existing anti-stick coating is coated on the surface of the high-frequency electric knife substrate, but has the problems of poor conductivity, weak anti-adhesion force and easy falling off.

[0006] The purpose of the present invention can be achieved through the following technical solutions: A method for preparing a low-temperature anti-stick coating for a high-frequency electric knife comprises at least the following preparation steps: Perform surface treatment and electrochemical polishing on the high-frequency electrosurgical knife substrate; Mechanically stirring hydrophobically modified ceramic powder, fusible polytetrafluoroethylene powder and silicone oil modified carbon nanotubes to obtain a mixed powder; The mixed powder is baked at 50-60° C. for 2-3 hours, and then sprayed on the surface of the electrochemically polished high-frequency electric knife substrate by an atmospheric plasma spraying process to obtain a low-temperature anti-stick coating.

[0007] As a further solution of the present invention: the mass ratio of the hydrophobic modified ceramic powder, the fusible polytetrafluoroethylene powder and the silicone oil modified carbon nanotube is 20-30:40-60:1.

[0008] As a further solution of the present invention: the particle size of the hydrophobically modified ceramic powder and the fusible polytetrafluoroethylene powder is 10-20 μm.

[0009] As a further solution of the present invention: the preparation method of the hydrophobically modified ceramic powder comprises the following steps: The silicone oil solution is added to the alumina powder and the titanium dioxide powder, and ultrasonically dispersed for 10-15 minutes, and then the catalyst is added, and ultrasonic dispersion is continued for 10-20 minutes. After the reaction is completed, the powder is dried to obtain a hydrophobically modified ceramic powder.

[0010] As a further solution of the present invention: the silicone oil solution is an acetone solution of terminal hydroxyl polydimethylsiloxane, and the mass ratio of the terminal hydroxyl polydimethylsiloxane to acetone is 0.6-0.8:100, and the catalyst is dibutyltin dilaurate or dioctyl dilaurate.

[0011] As a further embodiment of the present invention, the mass ratio of the silicone oil solution, the catalyst, the aluminum oxide powder and the titanium dioxide powder is 70-100:1-2:100:40-50.

[0012] As a further solution of the present invention: the preparation method of the silicone oil modified carbon nanotubes comprises the following steps: The multi-walled carbon nanotube material is added to dilute nitric acid, and then acidified and oxidized in an oil bath at 80°C. After the reaction is completed, the carbon nanotube material is filtered, washed with deionized water until neutral, and freeze-dried to obtain carboxyl-modified carbon nanotubes. The carboxylated carbon nanotubes are added to thionyl chloride, ultrasonically dispersed, N,N'-carbonyldiimidazole is added, and then amino mono-terminated polydimethylsiloxane is added, reacted at 60°C for 12-24h, filtered, washed, and dried to obtain silicone oil-modified carbon nanotubes.

[0013] As a further solution of the present invention: the mass ratio of the carboxylated carbon nanotubes, the N,N'-carbonyldiimidazole and the amino-terminated polydimethylsiloxane is 10:0.1-0.2:20-25.

[0014] As a further solution of the present invention: the material of the high-frequency electric knife is stainless steel, titanium alloy, tungsten alloy or hard alloy.

[0015] A low-temperature anti-stick coating for a high-frequency electric knife is prepared by any one of the preparation methods described above.

[0016] Beneficial effects of the present invention: The present invention uses hydrophobic modified ceramic powder, fusible polytetrafluoroethylene powder, and silicone oil modified carbon nanotubes to form a low-temperature anti-stick coating on the surface of a high-frequency electric knife, and the obtained high-frequency electric knife can be used at 40-70°C. Among them, the hydrophobic modified ceramic powder and the fusible polytetrafluoroethylene powder make the surface have good anti-stick properties, and the addition of carbon nanotubes makes the surface have good electrical conductivity, which can be applied to the surface of medical electrosurgical instruments that need to be discharged during use. The low-temperature anti-stick coating obtained by the method of the present invention has good electrical conductivity, anti-blood adhesion, anti-tissue adhesion, resistance to low-temperature storage, resistance to high-pressure steam sterilization and other properties, which can reduce the problems of tissue adhesion, eschar and the like generated by the medical high-frequency electric knife during use, and has a relatively broad application prospect in the medical field.

[0017] The ceramic particles and fusible polytetrafluoroethylene particles in the coating of the present invention are interlaced with each other, forming a micro-nano binary small papillary structure on the surface of the substrate, and there is a large amount of air in the gap of the protruding structure, so that the coating has excellent super-hydrophobicity, ensuring that the coating surface and the non-stickiness, scratch resistance, corrosion resistance, wettability and other properties of the coating surface and the coating are evenly distributed, that is, the coating has good hydrophobicity, good scratch resistance, good corrosion resistance and high coating adhesion. In addition, in the present invention, the ceramic particles are modified by terminal hydroxyl silicone oil, and the added carbon nanotube particles are modified by amino silicone oil. On the one hand, the silicone oil modification can improve the dispersibility of ceramic particles and carbon nanotubes, and on the other hand, it can increase the lubricity of the coating, reduce the viscosity, and reduce the shear force of the droplets on the coating surface, so that the coating surface has super slip and hydrophobicity, and the coating can also maintain good anti-sticking properties at low temperatures.

[0018] Before spraying the coating, the present invention uses an electrochemical polishing method to polish the surface of the high-frequency electric knife substrate to remove the oxides on the substrate surface and improve the flatness of the high-frequency electric knife surface, which is beneficial to improving the bonding strength of the coating on the substrate surface, so that the low-temperature anti-stick coating prepared by the present invention has better density, smooth and flat surface, and better surface strength. The polished high-frequency electric knife substrate is placed in a vacuum environment to avoid oxidation of the clean surface. The high-frequency electric knife substrate includes all common materials such as stainless steel, titanium alloy, tungsten alloy or cemented carbide. The preparation method of the present invention is applicable to various alloy substrates, and can have good bonding and anti-stick properties. DETAILED DESCRIPTION

[0019] The following will be described clearly and completely in conjunction with the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0020] Example 1 The preparation method of silicone oil modified carbon nanotubes comprises the following steps: 1 part by mass of multi-walled carbon nanotube material was added to dilute nitric acid, and acidified and oxidized in an oil bath at 80°C. After the reaction was completed, the carbon nanotube material was filtered, washed with deionized water until neutral, and freeze-dried to obtain carboxyl-modified carbon nanotubes. The above-mentioned carboxylated carbon nanotubes were ultrasonically dispersed in dimethyl sulfoxide, 0.1 parts by mass of N,N'-carbonyldiimidazole was added to activate the carboxyl groups of the carbon nanotubes, and then 2 parts by mass of amino mono-terminated polydimethylsiloxane were added and reacted at 60°C for 24 hours. The product was then filtered, washed and dried to obtain silicone oil-modified carbon nanotubes.

[0021] Example 2 The preparation method of hydrophobically modified ceramic powder comprises the following steps: A silicone oil solution in which 80 parts by mass of terminal hydroxyl polydimethylsiloxane and acetone have a mass ratio of 0.8:100 is added to 100 parts by mass of alumina powder and 40 parts by mass of titanium dioxide powder, and ultrasonically dispersed for 15 minutes. Then, 1 part by mass of catalyst dibutyltin dilaurate is added, and ultrasonic dispersion is continued for 20 minutes to obtain a uniform solution. The obtained solution is dried to obtain a hydrophobically modified ceramic powder.

[0022] Example 3 The preparation method of hydrophobically modified ceramic powder comprises the following steps: A silicone oil solution in which 100 parts by mass of terminal hydroxyl polydimethylsiloxane and acetone have a mass ratio of 0.8:100 is added to 100 parts by mass of alumina powder and 50 parts by mass of titanium dioxide powder, and ultrasonically dispersed for 15 minutes. Then, 1.2 parts by mass of catalyst dibutyltin dilaurate are added, and ultrasonic dispersion is continued for 20 minutes to obtain a uniform solution. The obtained solution is dried to obtain a hydrophobically modified ceramic powder.

[0023] Embodiment 4 The preparation method of the low-temperature anti-stick coating for high-frequency electric knife comprises the following steps: The high-frequency electrosurgical knife substrate was cleaned in an ultrasonic cleaning machine with anhydrous ethanol, acetone and water to complete the surface treatment, and then electrochemical polishing was performed. The current density of the electrochemical polishing was 0.6A / cm 2 During polishing, the electrolyte temperature is 80°C, the polishing time is 8 min, and the electrolyte is a mixture of sulfuric acid solution, phosphoric acid solution and polyethylene glycol; 25 parts by mass of the hydrophobic modified ceramic powder prepared in Example 2, 50 parts by mass of the fusible polytetrafluoroethylene powder and 1 part by mass of the silicone oil modified carbon nanotube prepared in Example 1 were mechanically stirred to obtain a mixed powder; The mixed powder was baked at 50°C for 2 hours and then sprayed on the surface of the high-frequency electric knife substrate after electrochemical polishing to obtain a low-temperature anti-stick coating.

[0024] Example 5 The preparation method of the low-temperature anti-stick coating for high-frequency electric knife comprises the following steps: The high-frequency electrosurgical knife substrate was cleaned in an ultrasonic cleaning machine with anhydrous ethanol, acetone and water to complete the surface treatment, and then electrochemical polishing was performed. The current density of the electrochemical polishing was 0.6A / cm 2 During polishing, the electrolyte temperature is 80°C, the polishing time is 8 min, and the electrolyte is a mixture of sulfuric acid solution, phosphoric acid solution and polyethylene glycol; 25 parts by mass of the hydrophobic modified ceramic powder prepared in Example 3, 50 parts by mass of the fusible polytetrafluoroethylene powder and 1 part by mass of the silicone oil modified carbon nanotube prepared in Example 1 were mechanically stirred to obtain a mixed powder; The mixed powder was baked at 50°C for 2 hours and then sprayed on the surface of the high-frequency electric knife substrate after electrochemical polishing to obtain a low-temperature anti-stick coating.

[0025] Example 6 The preparation method of the low-temperature anti-stick coating for high-frequency electric knife comprises the following steps: Perform surface treatment and electrochemical polishing on the high-frequency electrosurgical knife substrate; 30 parts by mass of the hydrophobic modified ceramic powder prepared in Example 2, 60 parts by mass of the fusible polytetrafluoroethylene powder and 1 part by mass of the silicone oil modified carbon nanotube prepared in Example 1 were mechanically stirred to obtain a mixed powder; The mixed powder was baked at 50°C for 3 hours and then sprayed on the surface of the high-frequency electric knife substrate after electrochemical polishing to obtain a low-temperature anti-stick coating.

[0026] Example 7 A method for preparing a low-temperature anti-stick coating for a high-frequency electric knife comprises the following steps: Perform surface treatment and electrochemical polishing on the high-frequency electrosurgical knife substrate; 30 parts by mass of the hydrophobic modified ceramic powder prepared in Example 3, 60 parts by mass of the fusible polytetrafluoroethylene powder and 1 part by mass of the silicone oil modified carbon nanotube prepared in Example 1 were mechanically stirred to obtain a mixed powder; The mixed powder was baked at 50°C for 3 hours and then sprayed on the surface of the high-frequency electric knife substrate after electrochemical polishing to obtain a low-temperature anti-stick coating.

[0027] Comparative Example 1 omits the preparation step of the hydrophobic modified ceramic powder. Compared with Example 4, Comparative Example 1 only replaces the hydrophobic modified ceramic powder prepared in Example 2 added in Example 4 with fusible polytetrafluoroethylene powder. The other components and preparation method are exactly the same as those in Example 4.

[0028] Comparative Example 2 Compared with Example 4, in Comparative Example 2, only the mass of the fusible polytetrafluoroethylene powder added in Example 4 is replaced by the hydrophobic modified ceramic powder prepared in Example 2, and the other components and preparation method are completely consistent with those of Example 4.

[0029] Comparative Example 3 omits the preparation steps of hydrophobically modified ceramic powder and silicone oil modified carbon nanotubes. Compared with Example 4, Comparative Example 3 replaces the hydrophobically modified ceramic powder prepared in Example 2 added in Example 4 with an unmodified mixed powder of alumina and titanium dioxide with a mass ratio of 5:1, and replaces the silicone oil modified carbon nanotubes prepared in Example 2 with an unmodified carbon nanotubes. The remaining components and preparation method are exactly the same as those in Example 4.

[0030] Comparative Example 4 A common medical high-frequency electric knife of model Sj-1 produced by Shaoxing Shangyu Xinyue Medical Instrument Co., Ltd. was selected.

[0031] Performance Testing Contact angle: The static contact angle of the coating was measured using a DSA30 contact angle meter produced by Kruess, Germany. The test results are shown in Table 1. Rolling angle: At room temperature, place the sample on a glass slide at an angle, drop a 10μL drop of water on it statically, and observe whether the water drop rolls on the sample. If it rolls, this angle is recorded as the rolling angle of the sample; if it does not roll, increase the number of glass slides until the water drop rolls on the sample. If the sample still does not roll at an angle of 90°, the rolling angle of the sample is recorded as 90°. The test results are shown in Table 1; Conductive performance: Place the two test pens of the digital multimeter at the center of the knife handle and the center of the knife head respectively to test the surface resistance of the knife. The test results are shown in Table 1. Anti-blood adhesion performance: The high-frequency electric knife in Examples 4-7 and Comparative Examples 1-4 was immersed in fresh pig blood, and the handle of the high-frequency electric knife was connected to a high-frequency power supply. The test was carried out at a power of 150 W. In each group of tests, the high-frequency electric knife was immersed in pig blood for 10 seconds, and the blood adhesion state was observed. The test results are shown in Table 1; Anti-tissue adhesion performance: The high-frequency electric knife in Examples 4-7 and Comparative Examples 1-4 was used to perform an electric cutting test on fresh pork at a power of 150 W. During the test, the electric knife was used to cut the pork surface from left to right, each cutting time was 5 seconds, and the cutting was repeated 3 times to observe the tissue adhesion state. The test results are shown in Table 1; Low-temperature anti-adhesive performance: The high-frequency electric knives in Examples 4-7 and Comparative Examples 1-4 were placed in a sealed sample bag and placed in an environmental chamber at 5°C for two weeks. The anti-adhesive blood performance was then tested. The test results are shown in Table 1.

[0032] Table 1: Statistical table of coating performance test data in Examples 4-7 and Comparative Examples 1-4

[0033] As can be seen from Table 1, the low-temperature anti-stick coating prepared by the present invention is attached to the surface of the substrate of the high-frequency electric knife, and the obtained coating has good conductivity and high hydrophobicity, and the high-frequency electric knife has good anti-blood adhesion, anti-tissue adhesion and low-temperature storage resistance. In Comparative Examples 1 and 2, the hydrophobic modified ceramic powder and the fusible polytetrafluoroethylene powder were not mixed for use, and the obtained low-temperature anti-stick coating had good hydrophobicity but poor anti-stick performance. In Comparative Example 3, the ceramic powder and carbon nanotubes were not modified with silicone oil, and the obtained high-frequency electric knife's anti-blood adhesion, anti-tissue adhesion and low-temperature storage resistance were not well improved. Comparative Example 4 is an ordinary high-frequency electric knife on sale, and its performance in all aspects is poor.

[0034] The above is a detailed description of an embodiment of the present invention, but the content is only a preferred embodiment of the present invention and cannot be considered to limit the scope of implementation of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the patent coverage of the present invention.

Claims

1. A method for preparing a low-temperature anti-stick coating for a high-frequency electric knife, characterized in that: The method comprises at least the following preparation steps: Perform surface treatment and electrochemical polishing on the high-frequency electrosurgical knife substrate; Mechanically stirring hydrophobically modified ceramic powder, fusible polytetrafluoroethylene powder and silicone oil modified carbon nanotubes to obtain a mixed powder; The mixed powder is baked at 50-60° C. for 2-3 hours, and then sprayed on the surface of the electrochemically polished high-frequency electric knife substrate by an atmospheric plasma spraying process to obtain a low-temperature anti-stick coating.

2. The method for preparing a low-temperature anti-stick coating for a high-frequency electric knife according to claim 1, characterized in that: The mass ratio of the hydrophobic modified ceramic powder, the fusible polytetrafluoroethylene powder and the silicone oil modified carbon nanotube is 20-30:40-60:

1.

3. The method for preparing a low-temperature anti-stick coating for a high-frequency electric knife according to claim 1, characterized in that: The particle size of the hydrophobic modified ceramic powder and the fusible polytetrafluoroethylene powder is 10-20 μm.

4. The method for preparing a low-temperature anti-stick coating for a high-frequency electric knife according to claim 1, characterized in that: The preparation method of the hydrophobically modified ceramic powder comprises the following steps: The silicone oil solution is added to the alumina powder and the titanium dioxide powder, and ultrasonically dispersed for 10-15 minutes, and then the catalyst is added, and ultrasonic dispersion is continued for 10-20 minutes. After the reaction is completed, the powder is dried to obtain a hydrophobically modified ceramic powder.

5. The method for preparing a low-temperature anti-stick coating for a high-frequency electric knife according to claim 4, characterized in that: The silicone oil solution is an acetone solution of terminal hydroxyl polydimethylsiloxane, and the mass ratio of the terminal hydroxyl polydimethylsiloxane to acetone is 0.6-0.8:

100. The catalyst is dibutyltin dilaurate or dioctyl dilaurate.

6. The method for preparing a low-temperature anti-stick coating for a high-frequency electric knife according to claim 5, characterized in that: The mass ratio of the silicone oil solution, the catalyst, the aluminum oxide powder and the titanium dioxide powder is 70-100:1-2:100:40-50.

7. The method for preparing a low-temperature anti-stick coating for a high-frequency electric knife according to claim 1, characterized in that: The method for preparing the silicone oil-modified carbon nanotubes comprises the following steps: The multi-walled carbon nanotube material is added to dilute nitric acid, and then acidified and oxidized in an oil bath at 80°C. After the reaction is completed, the carbon nanotube material is filtered, washed with deionized water until neutral, and freeze-dried to obtain carboxyl-modified carbon nanotubes. The carboxylated carbon nanotubes are added to thionyl chloride, ultrasonically dispersed, N,N'-carbonyldiimidazole is added, and then amino mono-terminated polydimethylsiloxane is added, reacted at 60°C for 12-24h, filtered, washed, and dried to obtain silicone oil-modified carbon nanotubes.

8. The method for preparing a low-temperature anti-stick coating for a high-frequency electric knife according to claim 7, characterized in that: The mass ratio of the carboxylated carbon nanotubes, the N,N'-carbonyldiimidazole and the amino-terminated polydimethylsiloxane is 10:0.1-0.2:20-25.

9. The method for preparing a low-temperature anti-stick coating for a high-frequency electric knife according to claim 1, characterized in that: The material of the high-frequency electric knife is stainless steel, titanium alloy, tungsten alloy or hard alloy.

10. A low-temperature anti-stick coating for high-frequency electric knife, characterized in that: Prepared by the preparation method described in any one of claims 1 to 9.

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