CN110075368B - A kind of preparation method of anti-sticking film on the surface of electric knife - Google Patents

A kind of preparation method of anti-sticking film on the surface of electric knife Download PDF

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CN110075368B
CN110075368B CN201910384271.4A CN201910384271A CN110075368B CN 110075368 B CN110075368 B CN 110075368B CN 201910384271 A CN201910384271 A CN 201910384271A CN 110075368 B CN110075368 B CN 110075368B
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简勇辉
费凛
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/08Materials for coatings
    • A61L31/082Inorganic materials
    • A61L31/088Other specific inorganic materials not covered by A61L31/084 or A61L31/086
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/14Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2420/00Materials or methods for coatings medical devices
    • A61L2420/02Methods for coating medical devices
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2420/00Materials or methods for coatings medical devices
    • A61L2420/08Coatings comprising two or more layers

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Abstract

The invention discloses a preparation method of an anti-sticking film layer on the surface of an electrotome, which comprises the steps of preparing a priming layer, arranging a conductive layer on the priming layer, and arranging an anti-sticking layer on the conductive layer to prepare the anti-sticking film layer; the bottom layer is an Ag layer, the conductive film layer is a mixed layer of SiO2 and Ag, and the anti-sticking layer is an Au or Ag film layer; preparing a SiO2 and Ag mixed layer with a nano-scale columnar matrix on the electrotome, and locking a large amount of air molecules between nano-columns of the mixed layer to ensure that most of the contact surface between small intestine tissues and the electrotome is air, namely generating an air cushion between the small intestine tissues and the electrotome, thereby achieving the purpose of adhesion prevention; the anti-sticking film layer prepared by the preparation method has low resistivity, high temperature resistance and oxidation resistance, meets the thermal shock test, and has small anti-sticking attenuation; in the process of hemostasis of the electrotome, the anti-sticking film layer prepared by the preparation method of the anti-sticking film layer on the surface of the electrotome ensures that the electrotome can not be adhered with a mucosa, avoids damaging the mucosa and ensures the hemostasis effect.

Description

一种电刀表面防粘粘膜层的制备方法A kind of preparation method of anti-sticking film on the surface of electric knife

技术领域technical field

本发明涉及一种膜层制备方法,尤其涉及的是一种电刀表面防粘粘膜层的制备方法。The invention relates to a method for preparing a film layer, in particular to a method for preparing an anti-sticking film layer on the surface of an electric knife.

背景技术Background technique

外科手术用的高频电刀的切割原理,是利用高频率的脉冲电火花对人体组织进行切割。具体的工作原理是:高频脉冲电源的两极分别接电刀和人体,当脉冲电压施加到电刀与小肠组织之间,将最近点的体液击穿,形成放电通道。由于通道的截面积很小,放电时间极短,致使能量高度集中,放电区域产生的瞬时高温,足以使局部的小肠组织熔断。第一次脉冲结束后,经过很短的时间间隔,第二个脉冲在另一个极间最近点击穿放电,熔断更深一层的小肠组织。如此周而复始地高频率循环下去,最终达到切除目标组织的效果。The cutting principle of the high-frequency electric knife used in surgery is to use high-frequency pulsed electric sparks to cut human tissue. The specific working principle is: the two poles of the high-frequency pulse power supply are respectively connected to the electrosurgical knife and the human body. When the pulse voltage is applied between the electrosurgical knife and the small intestine tissue, the body fluid at the nearest point is broken down to form a discharge channel. Due to the small cross-sectional area of the channel and the extremely short discharge time, the energy is highly concentrated, and the instantaneous high temperature generated in the discharge area is enough to fuse the local small intestinal tissue. After the end of the first pulse, after a short time interval, the second pulse taps through and discharges the nearest electrode between the other poles, fuses the deeper layer of small intestinal tissue. Such a high-frequency cycle is repeated over and over again, and finally the effect of removing the target tissue is achieved.

电刀在脉冲放电的过程中,有一部分电能量被释放到电刀上,电能迅速转化为热能,导致电刀温度上升。同时电刀与小肠组织之间是非接触放电,电刀的热能无法被小肠组织吸收;由于电刀体积很小,热容量也很小,在没有外界冷却液的情况下,电刀的温度可达到800℃以上(发红)。During the pulse discharge process of the electric knife, a part of the electric energy is released to the electric knife, and the electric energy is rapidly converted into heat energy, which causes the temperature of the electric knife to rise. At the same time, there is a non-contact discharge between the electrosurgical knife and the small intestine tissue, and the heat energy of the electrosurgical knife cannot be absorbed by the small intestinal tissue; because the electrosurgical knife is small in size and has a small heat capacity, the temperature of the electrosurgical knife can reach 800°C without external coolant. ℃ or higher (redness).

当发红的电刀与小肠组织再次接触时,可把脂肪和蛋白质瞬间碳化和变性;这些碳化变性的产物具有很强的粘附力,可把电刀牢牢地黏住,当强行拔出电刀时,往往会扯出一部分良好的小肠组织,产生新的创口,这样外科医生需要重新用电刀对新创口进行止血,但电刀有可能再次被黏住。When the reddened electric knife is in contact with the small intestinal tissue again, it can instantly carbonize and denature fat and protein; these carbonized and denatured products have strong adhesion, which can firmly stick the electric knife, and when it is forcibly pulled out During electrocautery, a part of the good intestinal tissue is often pulled out, creating a new wound, so the surgeon needs to re-use the electrocautery to stop the bleeding of the new wound, but the electrocautery may be stuck again.

为了解决电刀粘着的问题,在电刀上制备防粘涂层,是有效的解决途径之一。目前市面上的电刀多采用镀金或镀银等惰性金属,但效果欠佳。In order to solve the problem of electric knife sticking, it is one of the effective solutions to prepare anti-stick coating on the electric knife. At present, electrosurgical knives on the market mostly use inert metals such as gold-plated or silver-plated, but the effect is not good.

因此,亟待制备一种设置在电刀的电极头表面的膜层,可以较好地解决电刀电极头与小肠组织粘连的问题。Therefore, it is urgent to prepare a membrane layer disposed on the surface of the electrode tip of the electrosurgical knife, which can better solve the problem of adhesion between the electrode tip of the electrosurgical knife and the small intestine tissue.

发明内容SUMMARY OF THE INVENTION

本发明的目的在于提供一种电刀表面防粘粘膜层的制备方法,旨在解决现有的止血电极在表面镀金或镀银等惰性金属,小肠组织防粘效果欠佳的问题。The purpose of the present invention is to provide a preparation method of anti-sticking mucous layer on the surface of electric knife, aiming at solving the problem that the existing hemostatic electrode is plated with inert metal such as gold or silver on the surface, and the anti-sticking effect of small intestinal tissue is not good.

本发明的技术方案如下:一种电刀表面防粘粘膜层的制备方法,其中,制得的防粘粘膜层应用在高频电刀上,具体包括以下步骤:The technical scheme of the present invention is as follows: a preparation method of the anti-sticking film layer on the surface of an electric knife, wherein, the obtained anti-sticking film layer is applied on the high-frequency electric knife, and specifically comprises the following steps:

A1:制得打底层;A1: make the bottom layer;

A2:在打底层的表面制备纳米级柱状矩阵的导电层;A2: Prepare a conductive layer of nano-scale columnar matrix on the surface of the primer layer;

A3:在导电层的纳米柱顶端面设置防粘层,制得防粘粘膜层。A3: A release layer is provided on the top surface of the nano-pillars of the conductive layer to obtain a release film layer.

所述的电刀表面防粘粘膜层的制备方法,其中,所述打底层采用Ag材料层。In the preparation method of the anti-sticking film layer on the surface of the electric knife, wherein, the primer layer adopts an Ag material layer.

所述的电刀表面防粘粘膜层的制备方法,其中,所述导电层采用具有纳米级柱状矩阵的SiO2 和纳米Ag混合层。In the preparation method of the anti-sticking film layer on the surface of the electro-knife, the conductive layer adopts a mixed layer of SiO 2 and nano-Ag with a nano-scale columnar matrix.

所述的电刀表面防粘粘膜层的制备方法,其中,所述防粘层采用Ag材料层或Au材料层。In the preparation method of the anti-sticking film layer on the surface of the electric knife, wherein, the anti-sticking layer adopts an Ag material layer or an Au material layer.

所述的电刀表面防粘粘膜层的制备方法,其中,所述SiO2 和纳米Ag混合层具体包括以下组分:正硅酸四乙酯 12-16%;水 ≤1%;HCL ≤1%;NH4OH ≤1%;纳米银浆 1-5%;其余为无水乙醇。The preparation method of the anti-sticking film layer on the surface of the electric knife, wherein, the SiO 2 and nano-Ag mixed layer specifically includes the following components: tetraethyl orthosilicate 12-16%; water≤1%; HCL≤1 %; NH4OH ≤1%; nano-silver paste 1-5%; the rest are absolute ethanol.

所述的电刀表面防粘粘膜层的制备方法,其中,所述SiO2 和纳米Ag混合层采用溶胶-凝胶法制得。The preparation method of the anti-sticking film layer on the surface of the electric knife, wherein the SiO 2 and nano-Ag mixed layer is prepared by a sol-gel method.

所述的电刀表面防粘粘膜层的制备方法,其中,所述SiO2 和纳米Ag混合层的制备方法,包括以下步骤:The preparation method of the anti-sticking film layer on the surface of the electric knife, wherein, the preparation method of the SiO2 and nano-Ag mixed layer comprises the following steps:

a1:将正硅酸四乙酯缓慢滴加到水、盐酸、NH4OH和无水乙醇中,形成前驱体硅酸四乙酯;a1: slowly drop tetraethyl orthosilicate into water, hydrochloric acid, NH4OH and absolute ethanol to form the precursor tetraethyl silicate;

a2:将纳米银浆添加到前驱体硅酸四乙酯中,得到混合溶液;a2: adding the nano-silver paste to the precursor tetraethyl silicate to obtain a mixed solution;

a3:将混合溶液充分搅拌,并通过超声分散,得到SiO2 和纳米Ag混合湿凝胶。a3: The mixed solution is fully stirred and dispersed by ultrasonic to obtain a mixed wet gel of SiO2 and nano-Ag.

所述的电刀表面防粘粘膜层的制备方法,其中,所述纳米银浆的粒度为20-30nm。In the preparation method of the anti-sticking film layer on the surface of the electric knife, the particle size of the nano-silver paste is 20-30 nm.

所述的电刀表面防粘粘膜层的制备方法,其中,所述步骤a2中,纳米Ag的体积比为5-20 %。The preparation method of the anti-sticking film layer on the surface of the electric knife, wherein, in the step a2, the volume ratio of nano Ag is 5-20%.

所述的电刀表面防粘粘膜层的制备方法,其中,在止血头的表面首先电镀一层打底层,再在打底层的表面上用溶胶凝胶法制备一层纳米级柱状矩阵的导电层,最后在导电层的纳米柱顶端面电镀一层防粘层。The preparation method of the anti-sticking film layer on the surface of the electro-knife, wherein, a layer of primer is firstly electroplated on the surface of the hemostatic head, and then a conductive layer of a nano-level columnar matrix is prepared on the surface of the primer by a sol-gel method. , and finally a layer of anti-sticking layer is electroplated on the top surface of the nano-pillars of the conductive layer.

本发明的有益效果:本发明通过提供一种电刀表面防粘粘膜层的制备方法,制得打底层,将导电层设置在打底层上,将防粘层设置在导电层上,制得防粘粘膜层;所述打底层为Ag层,导电膜层为SiO2和Ag混合层,防粘层为Au或Ag膜层;在电刀上制备一层具有纳米级柱状矩阵的SiO2和Ag混合层,该混合层的纳米柱之间锁住大量的空气分子,使小肠组织与电刀之间的接触面大部分是空气,相当于在两者之间生成一层气垫,从而达到防粘的目的;本电刀表面防粘粘膜层的制备方法制得的防粘粘膜层具有低的电阻率,耐高温、抗氧化,满足热震试验,防粘性衰减很小;电刀在止血的过程中,本电刀表面防粘粘膜层的制备方法制得的防粘粘膜层保证电刀不会与粘膜粘连,避免伤害粘膜,保证止血效果。Beneficial effects of the present invention: The present invention provides a method for preparing an anti-sticking film layer on the surface of an electric knife to prepare a primer layer, a conductive layer is arranged on the primer layer, and an anti-stick layer is arranged on the conductive layer to prepare an anti-stick layer. Adhesive film layer; the bottom layer is Ag layer, the conductive film layer is SiO2 and Ag mixed layer, and the anti-adhesion layer is Au or Ag film layer; a layer of SiO2 and Ag mixed layer with nano-level columnar matrix is prepared on the electric knife , a large number of air molecules are locked between the nano-pillars of the mixed layer, so that most of the contact surface between the small intestine tissue and the electric knife is air, which is equivalent to generating a layer of air cushion between the two, so as to achieve the purpose of anti-sticking ; The anti-adhesion film layer obtained by the preparation method of the anti-adhesion film layer on the surface of the electric knife has low resistivity, high temperature resistance, anti-oxidation, meets the thermal shock test, and the anti-adhesive film attenuation is very small; The anti-adhesion mucous layer obtained by the preparation method of the anti-adhesion mucous layer on the surface of the electric knife ensures that the electric knife will not adhere to the mucous membrane, avoids damage to the mucous membrane, and ensures the hemostatic effect.

附图说明Description of drawings

图1是本发明中不粘粘膜的胃肠道内止血电刀的结构示意图。FIG. 1 is a schematic diagram of the structure of the non-stick mucosal hemostatic electrosurgical knife in the gastrointestinal tract of the present invention.

图2是本发明中电刀表面的防粘粘膜层的结构示意图。Figure 2 is a schematic structural diagram of the anti-adhesion film layer on the surface of the electrosurgical knife in the present invention.

图3是本发明中电刀表面防粘粘膜层的制备方法的步骤流程图。FIG. 3 is a flow chart of the steps of the preparation method of the anti-sticking film layer on the surface of the electric knife according to the present invention.

具体实施方式Detailed ways

为使本发明的目的、技术方案及优点更加清楚、明确,以下参照附图并举实施例对本发明进一步详细说明。In order to make the objectives, technical solutions and advantages of the present invention clearer and clearer, the present invention will be further described in detail below with reference to the accompanying drawings and examples.

如图1所示,一种不粘粘膜的胃肠道内止血电刀,包括控制端1和肠内工作端2,所述控制端1与肠内工作端2相接;所述的控制端1上设有通电接口12;所述的肠内工作端2包括肠内工作软管21和可伸缩的通电芯22,所述通电芯22安装在肠内工作软管21内;所述的通电芯22与通电接口12电连接;所述的通电芯22的尾端设有光滑的止血头220,在止血头220的表面设置有防粘粘膜层,所述防粘粘膜层包括依次设置在止血头220的表面的打底层31、导电层32和防粘层33(如图2所示),在止血头220的表面首先设置打底层31,再在打底层31的表面设置纳米级柱状矩阵的导电层32,最后在导电层32的纳米柱顶端面设置防粘层33。As shown in Figure 1, a non-stick mucosal gastrointestinal hemostatic electrosurgical knife includes a control end 1 and an intestinal working end 2, and the control end 1 is connected to the intestinal working end 2; the control end 1 There is an electrification interface 12 on it; the intestinal working end 2 includes an intestinal working hose 21 and a retractable electrification core 22, and the electrification core 22 is installed in the intestinal working hose 21; the electrification core 22 is electrically connected with the energizing interface 12; the tail end of the energizing core 22 is provided with a smooth hemostatic head 220, and an anti-sticking mucous layer is arranged on the surface of the hemostatic head 220, and the The bottom layer 31, the conductive layer 32 and the anti-stick layer 33 on the surface of the 220 (as shown in FIG. 2) are firstly provided with the bottom layer 31 on the surface of the hemostatic head 220, and then the conductive layer of the nano-level columnar matrix is set on the surface of the bottom layer 31. layer 32 , and finally a release layer 33 is provided on the top surface of the nano-pillars of the conductive layer 32 .

具体地,所述打底层31采用Ag材料层,厚度为3-8 µm;在止血头220表面与导电层32之间设置一层Ag材料过渡层,并高温热处理,可以使止血头220与Ag材料层之间、Ag材料层与导电层32之间生成热扩散的过渡层,从而提高了结合强度和抗热震性;所述Ag材料层的设置,可以提高与止血头220表面的结合强度,提高整个防粘粘膜层的抗热震性和导电性。Specifically, the primer layer 31 is made of an Ag material layer with a thickness of 3-8 μm; a transition layer of Ag material is arranged between the surface of the hemostatic head 220 and the conductive layer 32, and heat treatment at high temperature can make the hemostatic head 220 and Ag A thermally diffusing transition layer is formed between the material layers, between the Ag material layer and the conductive layer 32, thereby improving the bonding strength and thermal shock resistance; the setting of the Ag material layer can improve the bonding strength with the surface of the hemostatic head 220 , to improve the thermal shock resistance and electrical conductivity of the entire release film.

具体地,所述导电层32采用SiO2 和纳米Ag混合层,厚度为5-20µm。通过溶胶凝胶法在止血头220表面制备一层具有纳米级柱状矩阵的SiO2 和纳米Ag混合层,该混合层的纳米柱之间锁住大量的空气分子,使小肠组织与电刀之间的接触面大部分是空气,相当于在两者之间生成一层气垫,从而达到防粘的目的;SiO2 和纳米Ag混合层可以显著减少整个防粘粘膜层的电阻率、降低通电时整个防粘粘膜层自身的发热而导致的体积膨胀,从而使整个防粘粘膜层与止血头220的热膨胀系数更为匹配。Specifically, the conductive layer 32 is a mixed layer of SiO2 and nano-Ag, and the thickness is 5-20µm. A layer of SiO2 and nano-Ag mixed layer with nano-column matrix is prepared on the surface of the hemostatic head 220 by the sol-gel method. A large number of air molecules are locked between the nano-columns of the mixed layer, so that the gap between the small intestine tissue and the electrosurgical knife is reduced. Most of the contact surface is air, which is equivalent to generating a layer of air cushion between the two, so as to achieve the purpose of anti-sticking; the mixed layer of SiO2 and nano-Ag can significantly reduce the resistivity of the entire anti-sticking film layer and reduce the entire anti-sticking layer when energized. The volume expansion caused by the heating of the mucosal layer itself makes the thermal expansion coefficient of the entire anti-adhesive mucosal layer and the hemostatic head 220 more matched.

进一步地,所述SiO2 和纳米Ag混合层具体包括以下组分:正硅酸四乙酯(TEOS)12-16%;水 ≤1%;HCL(盐酸) ≤1%;NH4OH ≤1%;纳米银浆 1-5%;其余为无水乙醇。Further, the SiO2 and nano-Ag mixed layer specifically includes the following components: tetraethyl orthosilicate (TEOS) 12-16%; water≤1%; HCL (hydrochloric acid) ≤1%; NH4OH ≤1%; Silver paste 1-5%; the rest is absolute ethanol.

通过在前驱体正硅酸四乙酯(TEOS)里添加粒度为20-30nm的纳米银浆,使SiO2 和纳米Ag混合层具有良好的导电性和导热性,一方面满足了电刀高频放电的要求,另一方面减少了电刀基体与SiO2 和纳米Ag混合层的温差,从而提高了抗热震性和耐高温性。By adding nano-silver paste with a particle size of 20-30nm to the precursor tetraethyl orthosilicate (TEOS), the SiO2 and nano-Ag mixed layer has good electrical conductivity and thermal conductivity, on the one hand, it satisfies the high frequency discharge of electrosurgery. On the other hand, it reduces the temperature difference between the electrotome substrate and the SiO2 and nano-Ag mixed layer, thereby improving the thermal shock resistance and high temperature resistance.

具体地,所述防粘层33采用Ag材料层或Au材料层,厚度为0.5-2µm,因为防粘层33的厚度太薄,不能起到防粘的效果,如果防粘层33厚度太厚,则会使导电层32的纳米柱削峰平谷、失去微纳结构。所述Au、Ag是惰性金属,与蛋白质的亲和性都比SiO2更差,在SiO2 和纳米Ag混合层的纳米粗糙表面电镀一层薄薄Ag材料层或Au材料层,最终形成纳米级粗糙的Au或Ag膜,从而达到防粘的目的,所以Ag材料层或Au材料层可以防止止血头220在止血的同时与粘膜粘连,造成对粘膜的伤害。Specifically, the anti-adhesion layer 33 is made of Ag material layer or Au material layer, and the thickness is 0.5-2 μm. Because the thickness of the anti-adhesion layer 33 is too thin, the anti-adhesion effect cannot be achieved. If the thickness of the anti-adhesion layer 33 is too thick , the nano-pillars of the conductive layer 32 will be cut to peaks and valleys, and the micro-nano structures will be lost. The Au and Ag are inert metals, and their affinity with proteins is worse than that of SiO2. Electroplating a thin Ag material layer or Au material layer on the nano-rough surface of the SiO2 and nano-Ag mixed layer finally forms nano-roughness. Therefore, the Ag material layer or the Au material layer can prevent the hemostatic head 220 from adhering to the mucous membrane while hemostasis, thereby causing damage to the mucous membrane.

一种如上述所述的防粘粘膜层的制备方法,具体包括以下步骤:A preparation method of the above-mentioned anti-sticking film layer, specifically comprises the following steps:

A1:制得打底层31;A1: make the bottom layer 31;

A2:在打底层31的表面制备纳米级柱状矩阵的导电层32;A2: Prepare the conductive layer 32 of the nano-scale columnar matrix on the surface of the primer layer 31;

A3:在导电层32的纳米柱顶端面设置防粘层33,制得防粘粘膜层。A3: A release layer 33 is provided on the top surface of the nano-pillars of the conductive layer 32 to obtain a release film layer.

具体地,所述导电层32为纳米级柱状矩阵的SiO2 和纳米Ag混合层,所述SiO2 和纳米Ag混合层采用溶胶-凝胶法制得。Specifically, the conductive layer 32 is a mixed layer of SiO2 and nano-Ag in a nano-level columnar matrix, and the mixed layer of SiO2 and nano-Ag is prepared by a sol-gel method.

进一步地,所述SiO2 和纳米Ag混合层的制备方法,包括以下步骤:Further, the preparation method of the SiO2 and nano-Ag mixed layer includes the following steps:

a1:将正硅酸四乙酯(TEOS)缓慢滴加到水、盐酸、NH4OH和无水乙醇中,形成前驱体硅酸四乙酯;a1: Slowly add tetraethyl orthosilicate (TEOS) dropwise to water, hydrochloric acid, NH4OH and absolute ethanol to form the precursor tetraethyl silicate;

a2:将纳米银浆添加到前驱体硅酸四乙酯中,得到混合溶液;a2: adding the nano-silver paste to the precursor tetraethyl silicate to obtain a mixed solution;

a3:将混合溶液充分搅拌,并通过超声波充分分散,得到SiO2 和纳米Ag混合湿凝胶。a3: The mixed solution is fully stirred and fully dispersed by ultrasonic waves to obtain a mixed wet gel of SiO2 and nano-Ag.

其中,所述纳米银浆的粒度为20-30nm。Wherein, the particle size of the nano-silver paste is 20-30 nm.

其中,所述步骤a2中,纳米Ag的体积比为5-20 %。Wherein, in described step a2, the volume ratio of nano Ag is 5-20%.

一种将上述所述的防粘粘膜层设置在电刀表面的方法,具体包括以下步骤:A method for disposing the above-mentioned anti-sticking film layer on the surface of an electric knife, specifically comprising the following steps:

B1:将打底层31覆盖在整个止血头220的表面;B1: Cover the surface of the entire hemostatic head 220 with the primer layer 31;

B2:将纳米级柱状矩阵的导电层32覆盖在整个打底层31的表面;B2: covering the conductive layer 32 of the nanoscale columnar matrix on the entire surface of the bottom layer 31;

B3:对止血头220表面的打底层31和导电层32采用高温200-500℃烘烤2-4小时。一般的SiO2膜的烘烤工艺为120-200℃,0.5-1小时,本技术方案中采用高温200-500℃对打底层31和导电层32烘烤2-4小时,使各个界面(止血头220表面-Ag材料层、Ag材料层-SiO2 和纳米Ag混合层)之间相互热扩散,形成显著的过渡层,有效提高防粘粘膜层与止血头220表面的结合强度和抗热震性。B3: The primer layer 31 and the conductive layer 32 on the surface of the hemostatic head 220 are baked at a high temperature of 200-500° C. for 2-4 hours. The general baking process of the SiO2 film is 120-200°C for 0.5-1 hour. In this technical solution, a high temperature of 200-500°C is used to bake the bottom layer 31 and the conductive layer 32 for 2-4 hours, so that each interface (hemostatic head) is baked for 2-4 hours. 220 surface-Ag material layer, Ag material layer-SiO2 and nano-Ag mixed layer) are thermally diffused with each other to form a significant transition layer, which effectively improves the bonding strength and thermal shock resistance of the anti-adhesive film layer and the surface of the hemostatic head 220.

B4:将防粘层33覆盖在导电层32的纳米柱顶端面上。B4: Cover the top surface of the nano-pillars of the conductive layer 32 with the release layer 33 .

本技术方案现列举以下实施例加以说明:The technical scheme now enumerates the following examples to illustrate:

实施例1Example 1

打底层31:Ag材料层,厚度3µm。Bottom layer 31: Ag material layer with a thickness of 3µm.

导电层32:SiO2 和纳米Ag混合层,厚度20µm;其中,SiO2 和纳米Ag混合层的各个成分如下:正硅酸四乙酯(TEOS) 12%;水 1%;HCL 1%;NH4OH 1%;纳米银浆 1%;其余为无水乙醇。Conductive layer 32: a mixed layer of SiO2 and nano-Ag, with a thickness of 20 µm; the components of the mixed layer of SiO2 and nano-Ag are as follows: tetraethyl orthosilicate (TEOS) 12%; water 1%; HCL 1%; NH4OH 1% ; Nano silver paste 1%; the rest is absolute ethanol.

防粘层33:Ag材料层,厚度0.5µm。Release layer 33: Ag material layer, thickness 0.5µm.

所述SiO2 和纳米Ag混合层的制备:将12%正硅酸四乙酯(TEOS)缓慢滴加到1%水、1%盐酸、1%NH4OH和无水乙醇中,形成前驱体硅酸四乙酯;将1%纳米银浆添加到前驱体硅酸四乙酯中,得到混合溶液;将混合溶液充分搅拌,并通过超声分散,得到SiO2 和纳米Ag混合湿凝胶。其中,所述纳米银浆的粒度为20nm;所述步骤S2中,纳米Ag的体积比为5 µm。The preparation of the SiO2 and nano-Ag mixed layer: 12% tetraethyl orthosilicate (TEOS) was slowly added dropwise to 1% water, 1% hydrochloric acid, 1% NH4OH and absolute ethanol to form the precursor tetraethyl silicate. ethyl ester; adding 1% nano-silver paste to the precursor tetraethyl silicate to obtain a mixed solution; fully stirring the mixed solution and dispersing by ultrasonic to obtain a mixed wet gel of SiO2 and nano-Ag. Wherein, the particle size of the nano-silver paste is 20 nm; in the step S2, the volume ratio of the nano-Ag is 5 μm.

将防粘粘膜层设置在电刀表面:将Ag材料层电镀在整个止血头220的表面,厚度为3µm;将纳米级柱状矩阵的SiO2 和纳米Ag混合层涂覆在整个Ag材料层的表面,厚度为20µm;然后高温200℃烘烤4小时;将Ag材料层电镀在SiO2 和纳米Ag混合层的纳米柱顶端面上,厚度为0.5µm。Set the anti-adhesion film layer on the surface of the electrosurgical knife: electroplate the Ag material layer on the surface of the entire hemostatic head 220 with a thickness of 3 µm; coat the nano-scale columnar matrix of SiO2 and nano-Ag mixed layer on the entire surface of the Ag material layer, The thickness is 20µm; then it is baked at a high temperature of 200℃ for 4 hours; the Ag material layer is electroplated on the top surface of the nanopillars of the SiO2 and nano-Ag mixed layer with a thickness of 0.5µm.

实施例2Example 2

打底层31:Ag材料层,厚度8µm。Bottom layer 31: Ag material layer with a thickness of 8µm.

导电层32:SiO2 和纳米Ag混合层,厚度5µm;其中,SiO2 和纳米Ag混合层的各个成分如下:正硅酸四乙酯(TEOS) 16%;水 0.5%;HCL 0.5%;NH4OH 0.5%;纳米银浆 5%;其余为无水乙醇。Conductive layer 32: a mixed layer of SiO2 and nano-Ag, with a thickness of 5 µm; the components of the mixed layer of SiO2 and nano-Ag are as follows: tetraethyl orthosilicate (TEOS) 16%; water 0.5%; HCL 0.5%; NH4OH 0.5% ; Nano silver paste 5%; the rest is absolute ethanol.

防粘层33:Au材料层,厚度1µm。Release layer 33: Au material layer with a thickness of 1 µm.

所述SiO2 和纳米Ag混合层的制备:将16%正硅酸四乙酯(TEOS)缓慢滴加到0.5%水、0.5%盐酸、0.5%NH4OH和无水乙醇中,形成前驱体硅酸四乙酯;将5%纳米银浆添加到前驱体硅酸四乙酯中,得到混合溶液;将混合溶液充分搅拌,并通过超声分散,得到SiO2 和纳米Ag混合湿凝胶。其中,所述纳米银浆的粒度为30nm;所述步骤S2中,纳米Ag的体积比为20 µm。The preparation of the SiO2 and nano-Ag mixed layer: 16% tetraethyl orthosilicate (TEOS) was slowly added dropwise to 0.5% water, 0.5% hydrochloric acid, 0.5% NH4OH and absolute ethanol to form the precursor tetraethyl silicate. ethyl ester; adding 5% nano-silver paste to the precursor tetraethyl silicate to obtain a mixed solution; fully stirring the mixed solution and dispersing by ultrasonic to obtain a mixed wet gel of SiO2 and nano-Ag. Wherein, the particle size of the nano-silver paste is 30 nm; in the step S2, the volume ratio of the nano-Ag is 20 μm.

将防粘粘膜层设置在电刀表面:将Ag材料层电镀在整个止血头220的表面,厚度为8µm;将纳米级柱状矩阵的SiO2 和纳米Ag混合层涂覆在整个Ag材料层的表面,厚度为5µm;然后高温500℃烘烤2小时;将Ag材料层电镀在SiO2 和纳米Ag混合层的纳米柱顶端面上,厚度为1µm。Set the anti-adhesion film layer on the surface of the electrosurgical knife: electroplate the Ag material layer on the entire surface of the hemostatic head 220 with a thickness of 8 µm; coat the nano-scale columnar matrix of SiO2 and nano-Ag mixed layer on the entire surface of the Ag material layer, The thickness is 5µm; then it is baked at a high temperature of 500 °C for 2 hours; the Ag material layer is electroplated on the top surface of the nanopillars of the SiO2 and nano-Ag mixed layer with a thickness of 1µm.

实施例3Example 3

打底层31:Ag材料层,厚度5µm。Bottom layer 31: Ag material layer with a thickness of 5µm.

导电层32:SiO2 和纳米Ag混合层,厚度15µm;其中,SiO2 和纳米Ag混合层的各个成分如下:正硅酸四乙酯(TEOS) 16%;水 0.5%;HCL 0.5%;NH4OH 0.5%;纳米银浆 5%;其余为无水乙醇。Conductive layer 32: a mixed layer of SiO2 and nano-Ag, with a thickness of 15µm; the components of the mixed layer of SiO2 and nano-Ag are as follows: tetraethyl orthosilicate (TEOS) 16%; water 0.5%; HCL 0.5%; NH4OH 0.5% ; Nano silver paste 5%; the rest is absolute ethanol.

防粘层33:Au材料层,厚度0.8µm。Release layer 33: Au material layer, thickness 0.8µm.

所述SiO2 和纳米Ag混合层的制备:将14%正硅酸四乙酯(TEOS)缓慢滴加到0.8%水、0.8%盐酸、0.8%NH4OH和无水乙醇中,形成前驱体硅酸四乙酯;将3%纳米银浆添加到前驱体硅酸四乙酯中,得到混合溶液;将混合溶液充分搅拌,并通过超声分散,得到SiO2 和纳米Ag混合湿凝胶。其中,所述纳米银浆的粒度为25nm;所述步骤S2中,纳米Ag的体积比为15 µm。The preparation of the SiO2 and nano-Ag mixed layer: 14% tetraethyl orthosilicate (TEOS) was slowly added dropwise to 0.8% water, 0.8% hydrochloric acid, 0.8% NH4OH and absolute ethanol to form the precursor tetraethyl silicate. ethyl ester; adding 3% nano-silver paste to the precursor tetraethyl silicate to obtain a mixed solution; fully stirring the mixed solution and dispersing by ultrasonic to obtain a mixed wet gel of SiO2 and nano-Ag. Wherein, the particle size of the nano-silver paste is 25 nm; in the step S2, the volume ratio of the nano-Ag is 15 μm.

将防粘粘膜层设置在电刀表面:将Ag材料层电镀在整个止血头220的表面,厚度为5µm;将纳米级柱状矩阵的SiO2 和纳米Ag混合层涂覆在整个Ag材料层的表面,厚度为15µm;然后高温350℃烘烤3小时;将Ag材料层电镀在SiO2 和纳米Ag混合层的纳米柱顶端面上,厚度为0.8µm。Set the anti-adhesion film layer on the surface of the electrosurgical knife: electroplate the Ag material layer on the entire surface of the hemostatic head 220 with a thickness of 5 µm; coat the nano-scale columnar matrix SiO2 and nano-Ag mixed layer on the entire surface of the Ag material layer, The thickness is 15µm; then it is baked at a high temperature of 350 °C for 3 hours; the Ag material layer is electroplated on the top surface of the nanopillars of the SiO2 and nano-Ag mixed layer with a thickness of 0.8µm.

将实施例1-3的设置有防粘粘膜层的电刀分别进行电阻率测试、抗氧化实验、热震试验和防粘性衰减试验后,可以看出上述防粘粘膜层具有低的电阻率;耐800℃高温,防粘粘膜层不脱落、抗氧化;经过30-800℃热震试验,达到50-100次热震试验,防粘粘膜层不脱落;防粘粘膜层的防粘性衰减很小。After carrying out the resistivity test, anti-oxidation test, thermal shock test and anti-adhesion decay test of the electrosurgical knife provided with the anti-sticking film layer of Example 1-3 respectively, it can be seen that the above-mentioned anti-sticking film layer has low resistivity; Resistant to high temperature of 800 °C, the anti-adhesive film layer does not fall off and is anti-oxidative; after 30-800 °C thermal shock test, 50-100 thermal shock tests, the anti-adhesive film layer does not fall off; the anti-adhesive film layer has very little anti-adhesive attenuation .

本技术方案中,依次在电刀基体表面设置打底层31、导电膜层32和防粘层33,所述打底层31为Ag层,导电膜层32为SiO2和Ag混合层,防粘层33为Au或Ag膜层;设置打底层31目的是提高与电刀基体的结合强度,提高整个防粘粘膜层的抗热震性和导电性;设置导电膜层32可以显著减少整个防粘粘膜层的电阻率、降低通电时的整个防粘粘膜层自身的发热而导致的体积膨胀,从而使整个防粘粘膜层与电刀基体的热膨胀系数更为匹配;设置防粘层33是为了防止电刀在止血的同时与粘膜粘连,造成粘膜的伤害;在电刀上制备一层具有纳米级柱状矩阵的SiO2和Ag混合层,该混合层的纳米柱之间锁住大量的空气分子,使小肠组织与电刀之间的接触面大部分是空气,相当于在两者之间生成一层气垫,从而达到防粘的目的;通过在电刀基体表面设置打底层31、导电膜层32和防粘层33,不但实现了电刀导电止血的目的,还保证电刀不会与粘膜粘连,避免伤害粘膜,保证止血效果。In this technical solution, a primer layer 31, a conductive film layer 32 and an anti-stick layer 33 are sequentially arranged on the surface of the electro-knife base body, the primer layer 31 is an Ag layer, the conductive film layer 32 is a mixed layer of SiO2 and Ag, and the anti-stick layer 33 It is Au or Ag film layer; the purpose of setting the bottom layer 31 is to improve the bonding strength with the electrosurgery substrate, and improve the thermal shock resistance and electrical conductivity of the entire anti-adhesive film layer; setting the conductive film layer 32 can significantly reduce the entire anti-stick film layer. It reduces the volume expansion caused by the heating of the entire anti-adhesive film itself when energized, so that the thermal expansion coefficient of the entire anti-adhesive film and the electrosurgical base is more matched; the anti-adhesive layer 33 is provided to prevent At the same time of hemostasis, it adheres to the mucous membrane, causing damage to the mucous membrane; a layer of SiO2 and Ag mixed layer with nano-column matrix is prepared on the electrosurgical knife. Most of the contact surface with the electric knife is air, which is equivalent to generating a layer of air cushion between the two, so as to achieve the purpose of anti-sticking; The layer 33 not only achieves the purpose of the electrosurgical knife to conduct electricity to stop bleeding, but also ensures that the electrosurgical knife will not adhere to the mucous membranes, avoid damage to the mucous membranes, and ensure the hemostasis effect.

应当理解的是,本发明的应用不限于上述的举例,对本领域普通技术人员来说,可以根据上述说明加以改进或变换,所有这些改进和变换都应属于本发明所附权利要求的保护范围。It should be understood that the application of the present invention is not limited to the above examples. For those of ordinary skill in the art, improvements or transformations can be made according to the above descriptions, and all these improvements and transformations should belong to the protection scope of the appended claims of the present invention.

Claims (8)

1. The preparation method of the anti-sticking film layer on the surface of the electrotome is characterized in that the prepared anti-sticking film layer is applied to a high-frequency electrotome and specifically comprises the following steps:
a1: preparing a bottoming layer;
a2: preparing a conductive layer of a nano-scale columnar matrix on the surface of the priming layer;
a3: arranging an anti-sticking layer on the top end surface of the nano column of the conducting layer to prepare an anti-sticking film layer;
the conductive layer is made of SiO with a nano-scale columnar matrix2And a nano Ag mixed layer; the SiO2The raw materials of the mixed layer with the nano Ag comprise the following components: 12-16% of tetraethyl orthosilicate; water is less than or equal to 1 percent; HCL is less than or equal to 1 percent; NH4OH is less than or equal to 1 percent; 1-5% of nano silver paste; the balance of absolute ethyl alcohol.
2. The method for preparing the surface anti-sticking film layer of the electrotome according to claim 1, wherein the primer layer is made of an Ag material layer.
3. The method for preparing the anti-sticking film layer on the surface of the electrotome according to claim 1, wherein the anti-sticking layer is made of an Ag material layer or an Au material layer.
4. The method for preparing the surface anti-sticking film layer of the electrotome according to claim 1, wherein the SiO is2The mixed layer with the nano Ag is prepared by a sol-gel method.
5. The method for preparing the electrotome surface anti-sticking film layer according to claim 4, wherein the method for preparing the SiO2 and nano Ag mixed layer comprises the following steps:
a 1: slowly and dropwise adding tetraethyl orthosilicate into water, hydrochloric acid, NH4OH and absolute ethyl alcohol to form a precursor tetraethyl silicate;
a 2: adding nano silver paste into a precursor tetraethyl silicate to obtain a mixed solution;
a 3: and fully stirring the mixed solution, and performing ultrasonic dispersion to obtain the wet mixed gel of SiO2 and nano Ag.
6. The method for preparing the electrotome surface anti-sticking film layer according to claim 5, wherein the particle size of the nano silver paste is 20-30 nm.
7. The method for preparing the anti-sticking film layer on the electrotome surface according to claim 5, wherein the volume ratio of the nano silver in the nano silver paste is 5-20%.
8. The method for preparing the anti-sticking film layer on the surface of the electrotome according to claim 1, wherein a primer layer is firstly electroplated on the surface of the hemostatic tip, then a conductive layer of a nano-scale columnar matrix is prepared on the surface of the primer layer by a sol-gel method, and finally an anti-sticking layer is electroplated on the top end surface of the nano-column of the conductive layer.
CN201910384271.4A 2019-05-09 2019-05-09 A kind of preparation method of anti-sticking film on the surface of electric knife Expired - Fee Related CN110075368B (en)

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