CN117165918B - Electrode for electrosurgical instrument for reducing tissue eschar and preparation method thereof - Google Patents
Electrode for electrosurgical instrument for reducing tissue eschar and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of medical appliances, and discloses an electrode for an electrosurgical instrument for reducing tissue eschar and a preparation method thereof, wherein the electrode has a good tissue adhesion preventing effect, and comprises a stainless steel electrode body and a carbon-containing coating deposited on the electrode body, wherein the carbon-containing coating comprises the following elements in percentage by mass: 10 to 15 weight percent of C,35 to 53 wt percent of Fe,30 to 45 wt percent of Cr,1 to 4wt percent of Mn and 1 to 4.5 wt percent of Ni. The preparation method provided by the invention adopts a mode of forming the carbon-containing coating on the electrode surface by fractional deposition coating, so that the problems of complex process for transferring the coating and easiness in tearing, pollution and wrinkling of the coating film transfer are avoided, the problem that the coating thickness and uniformity are inconsistent when the coating is directly deposited on the electrode surface is solved, the yield and yield of the coated electrode are improved, and the production cost of the coated electrode is reduced.
Description
Technical Field
The invention relates to the technical field of medical appliances, in particular to an electrode for an electrosurgical instrument for reducing tissue eschar and a preparation method thereof.
Background
The electrosurgical instrument is surgical equipment which heats tissues when the tissues are contacted with the body through high-frequency current generated by the electrode tip, realizes separation and solidification of the tissues of the body, and achieves the purposes of cutting, hemostasis and the like, and comprises a high-frequency electrotome, a radio-frequency electrotome, an ion electrotome and the like.
The electrode that current electrosurgical instrument used is mostly stainless steel material, and the electrode of this kind of material itself resistance is great, and at electrosurgical operation in-process, the tissue of heating probably can adhere on the thermoelectric pole, and the adhesion tissue that electrode surface was not cleared away in time can form the carbonization tissue of growing thicker under the high temperature effect, has not only increased the resistance, has hindered the energy transmission to target tissue, leads to the electrode to become "dull", grow, cutting efficiency and operation precision to reduce, and the tissue is adhered with electrode surface in addition, and tissue adhesion are stronger, tear adjacent tissue easily when taking out the electrode and clear up, lead to unnecessary bleeding and tissue damage, reduce operation quality.
A current common solution to the problem of tissue adhesion is to add a conductive non-stick coating, such as a teflon (PTFE) coating, to the electrode surface of the electrosurgical instrument, but PTFE coatings have been demonstrated to gradually ablate and break down by the arc during use of the electrosurgical knife, losing anti-stick properties. Patent CN 113180819A discloses an electrode for electrosurgical instrument without adhesion, wherein a growth process is adopted to coat a thin film material coating with anti-adhesion, high conductivity and wear resistance on the end bit of the surface of a metal electrode of the electrosurgical instrument to realize the effect without adhesion, and the thin film material coating is one of graphene, carbon nano tube, carbon fiber, fiber-metal nano particle composite material and fiber-alloy nano particle composite material. In patent CN 113180819A, the preparation method of the coated electrode includes that after the coated material of graphene or carbon nanotube is prepared by chemical vapor deposition, the coated material is coated on the surface of the cleaned electrode by wet transfer, spin coating, drop coating, deposition and other processes, but the transfer process of the coated material of graphene or carbon nanotube after growth is not only complicated and time-consuming, but also can cause tearing, wrinkling, pollution and other damage of the coated film, the production process is complex, and the production cost of the electrode is high.
Chemical Vapor Deposition (CVD) is a process in which chemical gases or vapors react on the surface of a substrate to synthesize a coating or nanomaterial, and is the most widely used technique in the semiconductor industry for depositing a variety of materials. A great deal of research results prove that the CVD method is one of the best means for growing high-quality graphene films, but when the CVD method is used for depositing the coating, particularly in industrial mass production, many technical problems still exist, such as the thickness, uniformity and other characteristics of the coating are difficult to control stably.
Disclosure of Invention
In view of the above, the present invention provides an electrode for electrosurgical instrument capable of reducing tissue eschar, which has good effect of preventing tissue adhesion, and a preparation method of the electrode, which avoids the problems of complex process of transferring coating and easy tearing, pollution and wrinkling of coating film transfer, and solves the problems of inconsistent coating thickness and uniformity caused by directly depositing coating on the surface of the electrode, thereby improving the yield and yield of the coated electrode, and reducing the production cost of the coated electrode.
In order to achieve the above object, the present invention provides an electrode for an electrosurgical instrument capable of reducing tissue eschar, the electrode comprising a stainless steel electrode body and a carbon-containing coating deposited on the stainless steel electrode body, the carbon-containing coating comprising the following elements in mass percent: 10 to 15 weight percent of C,35 to 53 wt percent of Fe,30 to 45 wt percent of Cr,1 to 4wt percent of Mn and 1 to 4.5 wt percent of Ni.
The carbon-containing coating provided by the invention can effectively reduce the electrode resistance, thereby reducing the heat accumulation in the use process of the electrode and reducing the adhesion of tissues on the electrode, and meanwhile, the carbon-containing coating provided by the invention has strong hydrophobicity, so that the liquids such as blood, tissue fluid and the like are difficult to stay on the surface of the electrode, the adhesion of tissues in the tissue cutting process is greatly reduced, and the phenomenon that the residual tissues on the surface of the electrode are continuously heated to form eschar is avoided.
The invention further provides a preparation method of the electrode for the electrosurgical instrument, which comprises the following steps:
placing a stainless steel electrode body and a catalyst in a quartz frame, placing the quartz frame in a heating zone of chemical vapor deposition equipment, and introducing inert gas into the chemical vapor deposition equipment to empty gas in the equipment; the catalyst is selected from one or more of Fe, co and Ni powder;
step two, heating chemical vapor deposition equipment to 700-1300 ℃;
and thirdly, intermittently introducing reaction gas into the chemical vapor deposition equipment to carry out fractional deposition of the carbon-containing coating, wherein the reaction gas comprises hydrogen and carbon source gas, and the carbon source gas is one or more of hydrocarbon gases.
The preparation method comprises the steps of adopting a chemical vapor deposition method, taking a stainless steel electrode body as a growth substrate, taking one or more of Fe, co and Ni powder as a catalyst, intermittently introducing reaction gas into chemical vapor deposition equipment at the growth temperature of 700-1300 ℃, carrying out fractional deposition on the growth substrate to obtain the carbon-containing coating, and cooling the stainless steel electrode body to room temperature after the deposition is finished to obtain the electrode for the electrosurgical instrument; the reaction gas includes hydrogen and a carbon source gas selected from one or more of hydrocarbon gases. Fe. The transition metals such as Co, ni and the like have higher carbon dissolving capacity, certain carbide can be formed, carbon atoms have high diffusion rate in the transition metals, and the transition metals are used as catalysts to help decompose carbon source gases.
Further, in some embodiments of the present invention, the specific operation of the third step is: introducing hydrogen and carbon source gas into the chemical vapor deposition equipment for the first time, stopping introducing the hydrogen and the carbon source gas after 2-5min, standing for 2-4min, introducing the hydrogen and the carbon source gas into the chemical vapor deposition equipment for the second time, stopping introducing the hydrogen and the carbon source gas after 2-6min, standing for 2-4min, introducing the hydrogen and the carbon source gas into the chemical vapor deposition equipment for the third time, and stopping introducing the gas in the furnace and heating the furnace tube after 4-6 min; the volume flow ratio of the hydrogen to the carbon source gas in each vapor deposition is 1: (0.4-2.0); the ventilation of the hydrogen and the carbon source gas is third time > second time > first time.
The chemical vapor deposition equipment is selected from any one of a CVD tube furnace, a microwave plasma CVD equipment and a magnetron sputtering CVD equipment.
At present, most of electrode base materials of high-frequency electrotomes are stainless steel materials, when a carbon material coating is prepared on a stainless steel substrate by using a traditional CVD method, the conditions of completely inconsistent growth thickness and uniformity of the coating in the same reaction furnace can occur, and amorphous carbon is easily generated by gas phase reaction of a carbon source above a substrate in the reaction furnace, so that the pollution of amorphous carbon is often easily seen in the grown coating, the yield and the yield of the electrode of the carbon-containing coating prepared by the traditional CVD method are low, and the cost is high. In the technical scheme, the method for depositing the coating in batches is adopted, so that the full cracking of the carbon source gas is ensured, and the effect of controlling the uniform growth of the coating is achieved. More preferably, in the fractional deposition of the coating, a method of gradually increasing the ventilation rate is adopted, and the amount of hydrogen and carbon source gas introduced in each deposition increases with the increase of the deposition times, so that the coating grows in a process from sparse to dense, and the uniformity of the deposited coating is easier to control.
Further, in the fractional deposition of the coating, the growth time and ventilation of each deposited coating need to be controlled, because ventilation is set low, the growth time of the coating can be longer, insufficient growth or overgrowth is easy, and uniformity is difficult to control; if the ventilation is set high, the carbon source gas is easily cracked insufficiently to form more amorphous carbon, and the uniformity of the coating is difficult to control. Specifically, in the third step, hydrogen and carbon source gas are introduced at 300-700sccm for the first time, hydrogen and carbon source gas are stopped at 300-600sccm after 2-5min, hydrogen and carbon source gas are introduced at 600-1000sccm for the second time after 2-4min, hydrogen and carbon source gas are stopped at 700-1200sccm after 2-6min, hydrogen and carbon source gas are introduced at 1000-1800sccm for the third time after 2-4min, and furnace gas is stopped at 4-6 min.
Meanwhile, the preparation method of the invention takes the stainless steel electrode body as a growth matrix, and the electrode body material of the electrosurgical instrument is stainless steel, which contains alloy elements such as iron, carbon, silicon, manganese, phosphorus, sulfur, chromium, nickel, molybdenum and the like, and the stainless steel electrode can be used as a growth substrate of a carbon-containing coating and also has a catalytic effect on hydrocarbon gas pyrolysis deposition. The carbon obtained by pyrolysis of hydrocarbon gas permeates into the stainless steel matrix, so that the carbon-containing coating obtained by deposition comprises the following elements in percentage by mass: 10 to 15 weight percent of C,35 to 53 wt percent of Fe,30 to 45 wt percent of Cr,1 to 4wt percent of Mn and 1 to 4.5 wt percent of Ni. Experiments prove that the carbon-containing coating containing the elements with the composition content has excellent conductivity and strong hydrophobicity.
In the CVD deposition process of the carbon-containing coating, hydrogen is not only reducing gas, but also carrier gas and auxiliary gas, and the volume flow ratio of the hydrogen to the carbon source gas is controlled within 1: (0.4-2.0), so that smooth carbon production by cracking and dehydrogenation of the carbon source gas is ensured, and wrinkles generated by deposition of the coating can be reduced, deposition of amorphous carbon is reduced, the flatness of the coating is improved, and the quality of the electrode coating is improved.
The decomposition temperature of the carbon source gas determines the growth temperature of the coating, and the carbon source gas is selected from methane, acetylene and ethylene, so that the full growth of the coating at the growth temperature of 700-1300 ℃ is ensured. The carbon source gas can be one or more of hydrocarbon gases, such as methane, which can be used as carbon source gas alone or with acetylene at a mass ratio of 1:0.5-1.
Preferably, in some embodiments of the present invention, the electrode surface may be cleaned prior to vapor deposition of the coating to remove surface impurities and improve adhesion of the coating to the electrode surface, such as cleaning the stainless steel high frequency electrotome electrode with deionized water and alcohol.
Compared with the prior art, the invention has the following advantages:
1) The anti-sticking smoke-eliminating electrode provided by the invention improves the hydrophobicity of the electrode surface of an electrosurgical instrument, so that blood, tissue fluid and other liquids are difficult to stay on the electrode surface, adhesion and eschar of tissues in the process of tissue cutting are greatly reduced, the cleaning time can be effectively saved, the cleaning period can be prolonged, the smoothness of an operation flow is maintained, and the operation time is greatly shortened while the concentration degree of doctors is improved;
2) Because of the increase of the hydrophobicity of the electrode surface, the liquids such as blood, tissue fluid and the like are difficult to stay on the electrode surface, and the phenomenon that residual tissues on the electrode surface are continuously heated and burnt to form eschar is avoided;
3) The method for depositing the coating material on the surface of the electrode by adopting the chemical vapor deposition for multiple times avoids the problems of complex process for transferring the coating and easy tearing, pollution and wrinkling of the coating film transfer, solves the problems that the coating thickness and uniformity are inconsistent when the coating is directly deposited on the surface of the electrode, improves the yield and the yield of the coated electrode, reduces the production cost of the coated electrode, and is suitable for industrial mass production.
Drawings
FIG. 1 is an AFM image of the electrode surface of example 1;
fig. 2 is an SEM image of the electrode surfaces of examples 1 to 4;
FIG. 3 is an SEM image of the surface of a stainless steel electrode (UNS S30300) of a high frequency electrotome used in the example of the present application (the electron microscope working conditions of A are HV-5.00kv, mag-1000x, det-ETD, mode-SE, WD-6.4mm, and the electron microscope working conditions of B are HV-5.00kv, mag-15000x, det-ETD, mode-SE, WD-7.1 mm);
FIG. 4 is a comparison of the adhesion of fresh pork liver cut tissue of an uncoated stainless steel electrode tip to an electrode tip of example 1;
FIG. 5 is a photograph of an electrotome electrode (defective product) prepared in comparative example;
FIG. 6 is a photograph of the electrotome electrode (good product) prepared in example 1.
Detailed Description
In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further described in detail with reference to specific embodiments. It should be understood that these descriptions are merely provided for further explanation of the features and advantages of the present invention and are not intended to limit the scope of the claims.
It should be noted that:
1. the CVD equipment used in the following examples, comparative examples and comparative examples is a CVD tube furnace with a heating zone length of 800-1200mm and an outer diameter of 100-150mm, and is suitable for mass production;
2. the following examples, comparative examples and comparative examples were each obtained by applying a coating layer on the surface of a high-frequency electrotome electrode by a CVD vapor deposition method.
The high-frequency electrotome electrode was made of 303 austenitic stainless steel (UNS S30300) and contained alloy elements in the amounts shown in table 1 below.
TABLE 1 alloy element content Table (wt%) of UNS S30300 stainless steel
| C | Si | Mn | P | S | Cr | Ni | Mo |
| ≤0.15 | ≤1.00 | ≤2.00 | ≤0.20 | ≥0.15 | 17-19 | 8-10 | ≤0.6 |
Example 1:
a method for preparing an electrode for an electrosurgical instrument for reducing tissue eschar, which comprises the following steps:
s1, cleaning an electrode by deionized water and alcohol, putting the electrode into a quartz frame, putting 0.5g of Fe powder with the granularity of 80-100 mu m into the quartz frame, and fixedly putting the quartz frame into a furnace tube heating zone;
s2, starting a cleaning mode, and evacuating argon for 10min at a flow rate of 5000 sccm;
s3, after evacuation, adjusting the helium flow to 1000sccm, heating the furnace tube, heating the heating region to 1300 ℃ for 120min, and maintaining for 5min;
s4, introducing hydrogen and methane according to 700sccm, stopping introducing hydrogen and methane after reacting for 5min, adjusting the flow rate of the helium to 5000sccm, and maintaining for 4min; adjusting the flow rate of helium to 1000sccm, introducing hydrogen and methane according to 1200sccm, reacting for 6min, stopping introducing hydrogen and methane, adjusting the flow rate of helium to 5000sccm, and maintaining for 4min; and adjusting the flow rate of helium to 1000sccm, introducing hydrogen and methane according to 2000sccm, reacting for 6min, stopping introducing hydrogen and methane, stopping reacting, stopping heating the furnace tube, and taking out the high-frequency electrotome electrode in the furnace after the reaction furnace is cooled to room temperature to finish the preparation of the electrode.
Example 2:
a method for preparing an electrode for an electrosurgical instrument for reducing tissue eschar, which comprises the following steps:
s1, cleaning an electrode by deionized water and alcohol, putting the electrode into a quartz frame, putting 0.5g of Fe powder with the granularity of 80-100 mu m into the quartz frame, and fixedly putting the quartz frame into a furnace tube heating zone;
s2, starting a cleaning mode, and evacuating helium for 10min at a flow of 5000 sccm;
s3, after evacuation, adjusting the helium flow to 1000sccm, heating the furnace tube, heating the heating region to 700 ℃ for 120min, and maintaining for 5min;
s4, introducing hydrogen and acetylene according to 300sccm, stopping introducing hydrogen and acetylene after reacting for 2min, adjusting the flow rate of helium to 5000sccm, and maintaining for 2min; adjusting the flow rate of helium to 1000sccm, introducing hydrogen and acetylene according to 700sccm, reacting for 2min, stopping introducing hydrogen and acetylene, adjusting the flow rate of helium to 5000sccm, and maintaining for 2min; and adjusting the flow rate of helium to 1000sccm, introducing hydrogen and acetylene according to 1200sccm, reacting for 4min, stopping introducing hydrogen and acetylene, stopping the reaction, stopping heating the furnace tube, and taking out the high-frequency electrotome electrode in the furnace after the temperature of the reaction furnace is reduced to room temperature to finish the preparation of the electrode.
Example 3:
a method for preparing an electrode for an electrosurgical instrument for reducing tissue eschar, which comprises the following steps:
s1, cleaning an electrode by deionized water and alcohol, putting the electrode into a quartz frame, putting 0.5g of Fe powder with the granularity of 80-100 mu m into the quartz frame, and fixedly putting the quartz frame into a furnace tube heating zone;
s2, starting a cleaning mode, and evacuating helium for 10min at a flow of 5000 sccm;
s3, after evacuation, adjusting the helium flow to 1000sccm, heating a furnace tube, heating a heating zone to 1100 ℃ for 120min, and maintaining for 5min;
s4, introducing hydrogen and ethylene according to 600sccm, stopping introducing hydrogen and ethylene after reacting for 4min, adjusting the flow rate of helium to 5000sccm, and maintaining for 3min; adjusting the flow rate of helium to 1000sccm, introducing hydrogen and ethylene according to 1000sccm, reacting for 5min, stopping introducing hydrogen and ethylene, adjusting the flow rate of helium to 5000sccm, and maintaining for 3min; and adjusting the flow rate of helium to 1000sccm, introducing hydrogen according to 1500sccm and ethylene according to 1500sccm, stopping introducing hydrogen and ethylene after reacting for 5min, stopping reacting, stopping heating the furnace tube, and taking out the high-frequency electrotome electrode in the furnace after the temperature of the reaction furnace is reduced to room temperature to finish the preparation of the electrode.
Example 4:
a method for preparing an electrode for an electrosurgical instrument for reducing tissue eschar, which comprises the following steps:
s1, cleaning an electrode by deionized water and alcohol, putting the electrode into a quartz frame, putting 0.5g of Fe powder with the granularity of 80-100 mu m into the quartz frame, and fixedly putting the quartz frame into a furnace tube heating zone;
s2, starting a cleaning mode, and evacuating helium for 10min at a flow of 5000 sccm;
s3, after evacuation, adjusting the helium flow to 1000sccm, heating the furnace tube, heating the heating region to 900 ℃ for 120min, and maintaining for 5min;
s4, introducing hydrogen and carbon source gas according to 450sccm, reacting for 3min, stopping introducing the hydrogen and the carbon source gas, adjusting the flow rate of helium to 5000sccm, and maintaining for 2min; adjusting the flow rate of helium to 1000sccm, introducing hydrogen and carbon source gas according to 850sccm, reacting for 4min, stopping introducing hydrogen and carbon source gas, adjusting the flow rate of helium to 5000sccm, and maintaining for 2min; and adjusting the flow rate of helium to 1000sccm, introducing hydrogen and carbon source gas according to 1300sccm, reacting for 4min, stopping introducing hydrogen and carbon source gas, stopping reacting, stopping heating the furnace tube, and taking out the high-frequency electrotome electrode in the furnace after the reaction furnace is cooled to room temperature to finish the preparation of the electrode. The carbon source gas is a mixed gas of methane and acetylene with a mass ratio of 1:0.5.
Comparative example 1:
the procedure of example 1 was followed to apply a coating layer to the surface of a high-frequency electrotome electrode to obtain a coated electrode, which was different from example 1 in that: and S3, heating the heating area at the temperature of 1500 ℃.
Comparative example 2:
the procedure of example 2 was followed to apply a coating layer to the surface of a high-frequency electrotome electrode to obtain a coated electrode, which was distinguished from example 2 in that: and S3, heating the heating area at the temperature of 600 ℃.
The following tests were performed on the electrodes prepared in examples 1 to 4, the electrodes prepared in comparative examples 1 and 2, and the stainless steel electrode without coating treatment.
1. Atomic Force Microscope (AFM) detection
The thicknesses and roughness (Ra) of the coatings on the electrode surfaces prepared in examples 1 to 4 are shown in table 2 below, as measured by AFM.
TABLE 2 comparison of coating thicknesses and roughness Ra for each electrode surface
| Example 1 | Example 2 | Example 3 | Example 4 | Uncoated stainless steel electrode | |
| Coating thickness (nm) | 401.25 | 698.31 | 576.58 | 627.94 | 0 |
| Ra（nm） | 146.385 | 153.466 | 148.943 | 152.697 | 140-150 |
As can be seen from Table 2, the thickness of the coating on the electrode prepared in examples 1 to 4 was between 400 and 700nm, and the roughness was not much different from that of the stainless steel electrode of the high frequency electric knife. Since the thickness of 10 layers of graphene is 3.4nm, and the thickness of the coating deposited in examples 1 to 4 of the present application is 400 to 700nm, it can be determined that the coating materials deposited in examples 1 to 4 of the present application are not graphene. FIG. 1 is an AFM image of the electrode surface of example 1.
2. Electron scanning mirror (SEM) inspection
When the electrodes of examples 1 to 4, the electrolytic and uncoated stainless steel electrodes of comparative examples 1 and 2 were observed by using an electron scanning mirror, and referring to fig. 2 and 3, it can be seen that the electrode surfaces provided in examples 1 to 4 were loose and irregular, have more pores, are similar to porous metal materials, and have a significant difference from the surface morphology of the uncoated stainless steel electrode, indicating that the surfaces of the electrodes provided in examples 1 to 4 were coated with a coating similar to porous metal materials.
3. EDS energy spectrum analysis
EDS spectroscopy was performed on the electrode surfaces of the electrodes prepared in examples 1 to 4, the electrolysis prepared in comparative examples 1 and 2, and the uncoated stainless steel electrode using an electron scanning microscope, and the elemental distribution results of the electrode surfaces were obtained from the EDS spectroscopy, and the detection results are shown in Table 3 below.
TABLE 3 surface element content of each electrode (wt%)
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | Uncoated stainless steel electrode | |
| C | 15.06 | 10.03 | 12.75 | 12.38 | 21.33 | 7.52 | 0.12 |
| Fe | 35.18 | 53.13 | 42.36 | 43.13 | 25.24 | 66.16 | 69.11 |
| Cr | 45.13 | 30.78 | 38.96 | 38.85 | 50.09 | 14.82 | 18.21 |
| Mn | 3.12 | 4.03 | 1.04 | 2.89 | 1.18 | 5.83 | 1.67 |
| Ni | 1.01 | 3.012.03 | 4.52 | 2.5 | 1.42 | 5.67 | 9.13 |
| Si | 0.15 | 0 | 0.1 | 0.09 | 0.22 | 0 | 0.89 |
| P | 0.03 | 0 | 0.02 | 0.01 | 0.10 | 0 | 0.13 |
| S | 0.04 | 0 | 0.03 | 0.03 | 0.09 | 0 | 0.28 |
| Mo | 0.28 | 0 | 0.22 | 0.13 | 0.33 | 0 | 0.46 |
4. Conductivity detection
The sheet resistivities of the electrodes prepared in examples 1 to 4, the coated electrodes prepared in comparative examples 1 and 2, and the uncoated stainless steel electrodes were examined using a sheet resistance meter, and the resistivities of the respective electrodes (resistivity=sheet resistance value×film thickness) were calculated therefrom, and the results are shown in table 4 below.
TABLE 4 sheet resistance and resistivity comparison Table for electrode tips
| Square resistance (King/Kou) | Resistivity (. Q. Cm) | |
| Example 1 | 75.635 | 0.90762 |
| Example 2 | 75.97 | 0.91164 |
| Example 3 | 76.3 | 0.9156 |
| Example 4 | 75.64 | 0.9076 |
| Comparative example 1 | 133.09 | 1.597 |
| Comparative example 2 | 223.92 | 2.687 |
| Uncoated stainless steel electrode | 262000 | 5240 |
As can be seen from Table 4, the electrodes prepared in examples 1-4 and comparative examples 1-2 have significantly lower resistivity than the uncoated stainless steel electrode, and the electrodes prepared in examples 1-4 have further lower resistivity than comparative examples 1-2.
5. Detection of hydrophobicity of electrode surface coating
The electrodes prepared in examples 1 to 4, the electrolysis prepared in comparative examples 1 and 2, and the water contact angle and diiodomethane contact angle of the uncoated stainless steel electrode were examined using a contact angle meter, whereby the free energy of the electrode surface was calculated using Wu's equation, and specific data are shown in table 5 below.
TABLE 5 comparative hydrophobic Property of electrode tips
| Water contact angle (°) | Diiodomethane contact angle (°) | Surface free energy (mN/m) | |
| Example 1 | 95.91 | 49.43 | 35.14 |
| Example 2 | 91.85 | 49.68 | 38.29 |
| Example 3 | 94.86 | 49.52 | 36.23 |
| Example 4 | 93.15 | 49.60 | 37.17 |
| Comparative example 1 | 72.33 | 49.79 | 47.36 |
| Comparative example 2 | 65.84 | 49.88 | 48.92 |
| Uncoated stainless steel electrode | 59.56 | 49.91 | 49.14 |
As can be seen from table 5, the water contact angle of the electrodes prepared in examples 1 to 4 is significantly larger than that of the electrodes prepared in comparative examples 1 to 2 and the uncoated stainless steel electrode, and the free energy of the surface is lower, which proves that the coating deposited on the electrode surface in examples 1 to 4 greatly enhances the surface hydrophobicity of the stainless steel electrode, so that liquids such as blood and interstitial fluid are difficult to stay on the electrode surface.
6. Tissue cutting adhesion test
Fresh isolated pork liver is selected as an electrode cutting test material, three electrode tips of clean non-coated stainless steel electrode tips (303 stainless steel electrodes), electrode tips prepared in examples 1-4 and electrode tips prepared in comparative examples 1-2 are randomly selected, weighed by a micrometer, 120s cutting is performed by an 80W electric cutting mode which is commonly used by a clinician in operation, the cut tips are placed for 60s and then weighed for three times to obtain an average value, and the average tissue adhesion amount of each tip is calculated after repeating three groups of tests, as shown in the following table 6.
TABLE 6 tissue adhesion quality comparison Table for electrode tips
| Uncoated tool bit | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | |
| Tissue adhesion quality (mg) | 5.1 | 0.9 | 1.0 | 1.2 | 0.8 | 4.3 | 4.8 |
As can be seen from Table 6 above, the electrode tips of examples 1-4 reduced adhesion quality by 81% compared to the conventional uncoated tips, and had good release properties. Compared with the common uncoated cutter heads, the electrode cutter heads in the comparative examples 1-2 have the advantages that the tissue adhesion amount on the cutter heads is reduced slightly and the change is not obvious.
Fig. 4 shows the adhesion of the uncoated stainless steel electrode tip to the fresh pork liver cut tissue of the electrode tip of example 1, and shows that the surface tissue adhesion of the common uncoated electrode is large and tight, while the surface adhesion of the coated electrode of example 1 is small and sparse.
The medical gauze wetted by physiological saline is used for wiping the electrode, so that the uncoated electrode is difficult to clean, a large amount of eschar is remained after the electrode is forcefully wiped, and the electrode can be wiped cleanly only by using a special electric knife cleaning blade for multiple times of friction; the electrodes of comparative examples 1-2 remained a small amount of eschar after wiping, and were still difficult to clean with a hard wipe, and were wiped clean only by multiple rubs with a special electric blade; the electrodes of examples 1-4 were allowed to recover a clean state by rubbing the gauze. Therefore, the electrode provided by the invention greatly reduces tissue adhesion and eschar in the tissue cutting process, can effectively prolong the cleaning period, is convenient for cleaning, saves time, keeps the operation flow smooth, improves the concentration of doctors and greatly shortens the operation time.
7. Comparison of growth uniformity of coatings from different deposition processes
Comparative example:
the coated electrode of the high-frequency electrotome is prepared according to the following process steps:
s1, cleaning an electrode by deionized water and alcohol, putting the electrode into a quartz frame, putting 0.5g of Fe powder with the granularity of 80-100 mu m into the quartz frame, and fixedly putting the quartz frame into a furnace tube heating zone;
s2, starting a cleaning mode, and evacuating argon for 10min at a flow rate of 5000 sccm;
s3, after the argon is emptied, adjusting the flow of the argon to 1000sccm, heating a furnace tube, heating the heating region to 1300 ℃ for 120min, and maintaining for 5min;
s4, introducing hydrogen and methane according to 2000sccm, stopping introducing hydrogen and methane after reacting for 10-15min, stopping reacting, stopping heating the furnace tube, and taking out the high-frequency electrotome electrode in the furnace after the reaction furnace is cooled to room temperature.
A batch (50 pieces) of high-frequency electrotome electrodes were prepared according to the method of the comparative example, the number of qualified electrotome electrodes was 8, the number of qualified electrotome electrodes was 0, and as shown in FIG. 5, the uniformity of the coating on the electrotome electrodes produced according to the process steps of the comparative example was poor, the coating growth was inconsistent, for example, the coating near the ventilation end in the front of the furnace body could overgrow and be black, while the coating near the exhaust end was gold, silver or other colors, and the process of the comparative example was unstable.
The same procedure was followed in example 1, using 50 prepared high-frequency electrode electrodes as a batch, to obtain 49 qualified electrode electrodes, 43 qualified electrode electrodes, and high yield, and the electrode prepared in example 1 was good in coating quality, uniform and stable, as shown in fig. 6.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be defined by the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (6)
1. An electrode for an electrosurgical instrument, characterized by: the electrode comprises a stainless steel electrode body and a carbon-containing coating deposited on the stainless steel electrode body, wherein the carbon-containing coating comprises the following elements in percentage by mass:
10 to 15 weight percent of C,35 to 53 percent of wt percent of Fe,30 to 45 percent of wt percent of Cr,1 to 4 weight percent of Mn and 1 to 4.5 percent of wt percent of Ni.
2. A method of making an electrode for an electrosurgical instrument as recited in claim 1, wherein: the method comprises the following steps:
placing a stainless steel electrode body and a catalyst in a quartz frame, placing the quartz frame in a heating zone of chemical vapor deposition equipment, and introducing inert gas into the chemical vapor deposition equipment to empty gas in the equipment; the catalyst is selected from one or more of Fe, co and Ni powder;
step two, heating chemical vapor deposition equipment to 700-1300 ℃;
step three, intermittently introducing reaction gas into the chemical vapor deposition equipment to carry out fractional deposition of the carbon-containing coating, wherein the reaction gas comprises hydrogen and carbon source gas, and the carbon source gas is one or more of hydrocarbon gases; the fractional deposition is specifically as follows: introducing hydrogen and carbon source gas into the chemical vapor deposition equipment according to 300-700sccm for the first time, stopping introducing the hydrogen and the carbon source gas after 2-5min, standing for 2-4min, introducing the hydrogen and the carbon source gas into the chemical vapor deposition equipment according to 700-1200sccm for the second time, stopping introducing the hydrogen and the carbon source gas after 2-6min, standing for 2-4min, introducing the hydrogen and the carbon source gas into the chemical vapor deposition equipment according to 1200-2000sccm for the third time, and stopping introducing the gas in the furnace and heating the furnace tube after 4-6 min; the ventilation of the hydrogen and the carbon source gas is third time > second time > first time.
3. A method of producing an electrode for an electrosurgical instrument according to claim 2, wherein: the volume flow ratio of the hydrogen to the carbon source gas in the reaction gas is 1: (0.4-2.0).
4. A method of producing an electrode for an electrosurgical instrument according to claim 2, wherein: the hydrocarbon gas includes methane, acetylene and ethylene.
5. A method of producing an electrode for an electrosurgical instrument according to claim 2, wherein: in the fractional deposition, the flow rate of the reaction gas introduced into each deposition increases with the increase of the deposition times.
6. A method of producing an electrode for an electrosurgical instrument according to claim 2, wherein: the chemical vapor deposition equipment is selected from any one of a CVD tube furnace, a microwave plasma CVD equipment and a magnetron sputtering CVD equipment.
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