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CN203498467U - Device for depositing film on internal surface of long pipe by using plasma enhanced chemical vapor deposition - Google Patents

Device for depositing film on internal surface of long pipe by using plasma enhanced chemical vapor deposition Download PDF

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CN203498467U
CN203498467U CN201320467293.5U CN201320467293U CN203498467U CN 203498467 U CN203498467 U CN 203498467U CN 201320467293 U CN201320467293 U CN 201320467293U CN 203498467 U CN203498467 U CN 203498467U
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vacuum chamber
plasma
chemical vapor
vapor deposition
power supply
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赵彦辉
于宝海
肖金泉
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Institute of Metal Research of CAS
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Abstract

本实用新型属于材料表面改性领域,涉及一种用等离子体增强化学气相沉积在长管内表面沉积薄膜的装置,解决现有PECVD方法在管内轴向等离子体放电的不均匀性,而且直接造成管内表面轴向薄膜沉积均匀性差等问题。在待处理的细长金属管置于管型真空室内,在金属管状工件的中心轴向放置一钨丝电极,向金属管内通入工作气体,在钨丝电极与真空室壁之间施加直流脉冲或射频信号,激励放电以产生等离子体。在真空室外缠绕漆包线构成电磁线圈,电磁线圈接直流稳压电源以产生电磁场。利用磁场对等离子体束流进行约束和控制,从而实现等离子体在管内壁均匀沉积薄膜的目的,适用于作为服役表面的管状工件的内壁表面镀膜。

The utility model belongs to the field of material surface modification, and relates to a device for depositing thin films on the inner surface of a long tube by using plasma enhanced chemical vapor deposition, which solves the inhomogeneity of the axial plasma discharge in the tube in the existing PECVD method, and directly causes Problems such as poor uniformity of surface axial film deposition. The slender metal tube to be processed is placed in a tubular vacuum chamber, a tungsten wire electrode is placed axially in the center of the metal tubular workpiece, the working gas is introduced into the metal tube, and a DC pulse is applied between the tungsten wire electrode and the wall of the vacuum chamber or radio frequency signal to stimulate the discharge to generate plasma. The enameled wire is wound outside the vacuum chamber to form an electromagnetic coil, and the electromagnetic coil is connected to a DC regulated power supply to generate an electromagnetic field. The magnetic field is used to confine and control the plasma beam, so as to achieve the purpose of uniformly depositing a thin film on the inner wall of the tube by the plasma, and is suitable for coating the inner wall surface of the tubular workpiece as the service surface.

Description

用等离子体增强化学气相沉积在长管内表面沉积薄膜装置Device for Depositing Thin Films on the Inner Surface of Long Tubes by Plasma-Enhanced Chemical Vapor Deposition

技术领域:Technical field:

本实用新型属于材料表面改性领域,涉及一种用等离子体增强化学气相沉积在长管内表面沉积薄膜的装置。The utility model belongs to the field of material surface modification, and relates to a device for depositing thin films on the inner surface of long tubes by using plasma enhanced chemical vapor deposition.

背景技术:Background technique:

在工业应用中有大量金属工件的内表面需要改性处理,特别是对于管件,例如油田上的抽油泵泵筒、输油管道、化工管道、汽车汽缸套,以及军事领域,特别是海军舰艇上配置的舰炮炮管以及鱼雷发射管等在恶劣环境下工作的内壁亟待强化处理的管状零部件,普通处理方法无法满足其表面强化要求。这些工件常因内壁磨损、腐蚀、氧化而发生早期失效,因此开发具有抗磨损、抗腐蚀、抗氧化的表面改性技术及工艺,是目前表面改性领域急需解决的难题。In industrial applications, the inner surface of a large number of metal workpieces needs to be modified, especially for pipe fittings, such as oil pump barrels on oil fields, oil pipelines, chemical pipelines, automobile cylinder liners, and military fields, especially on naval ships. For naval gun barrels, torpedo tubes, and other tubular parts whose inner walls need to be strengthened in harsh environments, ordinary treatment methods cannot meet the surface strengthening requirements. These workpieces often fail early due to inner wall wear, corrosion, and oxidation. Therefore, the development of surface modification technologies and processes with anti-wear, anti-corrosion, and anti-oxidation is an urgent problem in the field of surface modification.

相比于工件的外表面而言,管状工件内壁改性处理主要存在以下几个技术难题:一是受到内腔形状和尺寸的限制,一些处理方法很难实施,或者是即使能实施也很难得到良好的改性效果,尤其是对于一些细长的管件更是如此。二是受到内腔形状和尺寸的限制,一些处理介质很难进入管腔内部,或者是即使进入也难以保证改性层的均匀性。三是受到内腔形状和尺寸的限制,改性层与管壁的结合强度不高,限制了其使役性能的发挥。Compared with the outer surface of the workpiece, the modification of the inner wall of the tubular workpiece mainly has the following technical problems: First, due to the limitation of the shape and size of the inner cavity, some treatment methods are difficult to implement, or even if it can be implemented, it is difficult A good modification effect is obtained, especially for some slender pipes. Second, limited by the shape and size of the lumen, it is difficult for some treatment media to enter the lumen, or even if it enters, it is difficult to ensure the uniformity of the modified layer. Third, limited by the shape and size of the inner cavity, the bonding strength between the modified layer and the pipe wall is not high, which limits the performance of its service performance.

对于金属管内壁改性,最早人们提出用电镀和化学镀进行处理。但是化学镀由于常常使用有害化学药品,对环境有害,且镀层致密性较差;电镀尽管减少使用有害的化学药品,且镀层致密性优于化学镀,但是仍存在使用过程中结合较差而易剥落的问题。For the modification of the inner wall of metal pipes, it was first proposed to use electroplating and electroless plating for treatment. However, electroless plating is harmful to the environment due to the frequent use of harmful chemicals, and the compactness of the coating is poor; although electroplating reduces the use of harmful chemicals, and the compactness of the coating is better than that of electroless plating, it still has poor bonding during use and is easy to Peeling problem.

化学气相沉积(CVD)方法由于采用气体介质,更易于沉积复杂形状的工件,只要工件浸没在工作气体中即可在表面沉积所需薄膜。管状工件内表面镀膜正是利用CVD方法的这一特性,而且提出了一些改进方法,包括各种等离子体增强CVD(PECVD)方法。所沉积薄膜多为类金刚石膜(DLC)或TiN膜,利用这些硬质薄膜的高硬度、耐磨损、抗腐蚀性能,增加了工件的使用寿命。The chemical vapor deposition (CVD) method is easier to deposit workpieces with complex shapes due to the use of gas media. As long as the workpiece is immersed in the working gas, the desired film can be deposited on the surface. The coating on the inner surface of the tubular workpiece is just using this characteristic of the CVD method, and some improved methods have been proposed, including various plasma-enhanced CVD (PECVD) methods. Most of the deposited films are diamond-like carbon (DLC) or TiN films. The high hardness, wear resistance and corrosion resistance of these hard films are used to increase the service life of the workpiece.

乌拉圭的艾利特斯股份公司公布了一种用于等离子体增强化学气相沉积的等离子体系统(等离子体系统.发明专利:200880127994.6),该系统以待处理管件作为真空室,在管内插入一个同轴电极,在电极和管壁之间施加高频场、微波场、脉冲能量场、RF场、CC场、AC场等,将真空室内通入的气体离化以产生等离子体,从而实现在管内表面沉积薄膜。该系统的优点在于直接以被处理管件作为真空室,管外壁不需要特殊处理,且不需要庞大的等离子体反应器且便于携带。但管内壁薄膜均匀性仍待改善。Uruguay's Elites Co., Ltd. announced a plasma system for plasma-enhanced chemical vapor deposition (plasma system. Invention patent: 200880127994.6). The system uses the tube to be processed as a vacuum chamber and inserts a same Axial electrode, applying high-frequency field, microwave field, pulse energy field, RF field, CC field, AC field, etc. between the electrode and the tube wall, ionizes the gas introduced into the vacuum chamber to generate plasma, so as to achieve in-tube Thin films deposited on the surface. The advantage of this system is that the treated tube is directly used as a vacuum chamber, the outer wall of the tube does not need special treatment, and it does not require a huge plasma reactor and is easy to carry. However, the uniformity of the film on the inner wall of the tube still needs to be improved.

中国航天科技集团公司第五研究院第五一〇研究所的熊玉卿等人提出了一种在细长管道内壁镀制薄膜的方法(一种在细长管道内壁镀制薄膜的方法.发明专利:201110283626.4),该方法是将需镀膜的管道置于反应室内,将气相前驱体以脉冲形式交替通入反应器,第一种前驱体到达管道内后,以化学吸附在管道内壁形成一个单吸附层;再通入第二种前驱体,与第一种前驱体反应,在管道内壁生成一个单原子层的薄膜。在每个前驱体脉冲之间需用惰性气体进行清洗,再重复吸附和反应过程,逐层生成薄膜。该方法可在细长管道内壁镀制各种金属、氧化物、氮化物等各类薄膜材料,但是其薄膜与基体仅以化学吸附结合,结合力较差,且薄膜厚度较薄。Xiong Yuqing and others from the 510th Research Institute of the Fifth Research Institute of China Aerospace Science and Technology Corporation proposed a method of coating thin films on the inner walls of slender pipes (a method of coating thin films on the inner walls of slender pipes. Invention patent: 201110283626.4), the method is to place the pipe to be coated in the reaction chamber, and alternately pass the gas-phase precursor into the reactor in the form of pulses. After the first precursor reaches the pipe, it will be chemically adsorbed on the inner wall of the pipe to form a single adsorption layer. ; Then feed the second precursor to react with the first precursor to form a monoatomic layer film on the inner wall of the pipeline. Inert gas cleaning is required between each precursor pulse, and the adsorption and reaction process is repeated to form thin films layer by layer. This method can plate various metals, oxides, nitrides and other film materials on the inner wall of the slender pipe, but the film and the substrate are only combined by chemical adsorption, the bonding force is poor, and the film thickness is relatively thin.

德国的拉尔夫·斯坦也公布了一种等离子体辅助化学气相沉积方法与装置(在中空主体的内壁上进行等离子体辅助化学气相沉积的方法与装置.发明专利:200780026008.3),是将待处理的中空主体放入真空室,大面积的射频电极放置于真空室内部,将气燃喷枪放入中空主体内,通入气体后,通过向RF电极施加射频电场,点燃等离子体腔,在气燃喷枪的尖端形成等离子云,实现在中空主体内壁镀膜。该装置可以沉积DLC、TiOx、SiO2等镀层,但由于气燃喷枪外径的限制,不能出来内径低于20mm的管件内壁镀膜。Ralph Stein of Germany also announced a plasma-assisted chemical vapor deposition method and device (a method and device for plasma-assisted chemical vapor deposition on the inner wall of a hollow body. Invention patent: 200780026008.3), which is to be processed The hollow main body is placed in the vacuum chamber, and the large-area radio frequency electrode is placed inside the vacuum chamber. The gas-fuel spray gun is placed in the hollow main body. After the gas is introduced, the plasma chamber is ignited by applying a radio-frequency electric field to the RF electrode. The tip forms a plasma cloud to achieve coating on the inner wall of the hollow body. The device can deposit DLC, TiO x , SiO 2 and other coatings, but due to the limitation of the outer diameter of the gas-fired spray gun, the coating on the inner wall of the pipe with an inner diameter of less than 20mm cannot be produced.

大连理工大学的温小琼、王德真发明了一种用直流辉光放电在细长金属管内壁沉积类金刚石膜的方法(发明专利:200610200503.9),该方法在细长金属管的轴线上设置一根钨丝,与金属管构成同轴电极。钨丝作为阳极,在真空室内通入气体,在金属管上加恒定直流负偏压,在阳极钨丝的周围形成强电场区域,引起气体放电,从而在整个金属管内产生稳定的圆筒状的直流辉光等离子体,实现在金属管内表面均匀沉积类金刚石薄膜的目的。该方法可以处理直径5mm以上、长度5~2000mm的金属管内表面沉积类金刚石薄膜,沉积薄膜的种类有限,且膜基结合力仍待改善。Wen Xiaoqiong and Wang Dezhen from Dalian University of Technology invented a method of depositing a diamond-like film on the inner wall of a slender metal tube by DC glow discharge (invention patent: 200610200503.9). This method sets a tungsten wire on the axis of the slender metal tube , form a coaxial electrode with the metal tube. The tungsten wire is used as the anode, and the gas is passed into the vacuum chamber, and a constant DC negative bias is applied to the metal tube to form a strong electric field area around the anode tungsten wire, causing gas discharge, thereby producing a stable cylindrical shape in the entire metal tube. DC glow plasma achieves the purpose of uniformly depositing diamond-like film on the inner surface of the metal tube. The method can process the deposition of diamond-like films on the inner surface of metal tubes with a diameter of more than 5 mm and a length of 5-2000 mm. The types of deposited films are limited, and the bonding force of the film base still needs to be improved.

以色列公布了一项采用化学气相沉积在管内壁沉积涂层的方法(US4764398)(Method of depositing coatings on the inner surface of a tube by chemical vapordeposition),并获得美国专利,但其主要用于沉积太阳能吸收涂层。Israel announced a method of depositing coatings on the inner surface of a tube by chemical vapor deposition (US4764398) (Method of depositing coatings on the inner surface of a tube by chemical vapordeposition), and obtained a US patent, but it is mainly used for depositing solar energy absorption coating.

尽管PECVD在一定程度上解决了管内壁改性处理的技术难题,使得改性质量得到了很大改善,但仍存在一些问题有待解决。尤其是当管的内径变得越来越小或者长度变得越来越大时,辉光放电就会变得越来越难维持在管内部。在某些点处,即使一个中心电极被插入来促进等离子体的稳定性,等离子体甚至也会跳到管外面。这不仅影响了管内轴向等离子体放电的均匀性,而且直接造成管内表面轴向薄膜沉积均匀性差的难题。Although PECVD has solved the technical problems of the modification of the inner wall of the tube to a certain extent, and the quality of the modification has been greatly improved, there are still some problems to be solved. Especially as the inner diameter of the tube becomes smaller or the length becomes larger, the glow discharge becomes more and more difficult to maintain inside the tube. At some point, the plasma even jumped outside the tube, even though a center electrode was inserted to promote plasma stability. This not only affects the uniformity of the axial plasma discharge in the tube, but also directly causes the poor uniformity of the axial film deposition on the inner surface of the tube.

实用新型内容:Utility model content:

本实用新型的目的在于提供一种用等离子体增强化学气相沉积在长管内表面沉积薄膜的方法,解决现有PECVD方法在管内轴向等离子体放电的不均匀性,而且直接造成管内表面轴向薄膜沉积均匀性差等问题。The purpose of this utility model is to provide a method for depositing a film on the inner surface of a long tube by plasma enhanced chemical vapor deposition, which solves the inhomogeneity of the axial plasma discharge in the tube in the existing PECVD method, and directly causes the axial film on the inner surface of the tube Problems such as poor deposition uniformity.

本实用新型的技术方案是:The technical scheme of the utility model is:

一种用等离子体增强化学气相沉积在长管内表面沉积薄膜装置,采用磁场增强的等离子体增强化学气相沉积装置。A plasma-enhanced chemical vapor deposition device for depositing thin films on the inner surface of a long tube adopts a magnetic field-enhanced plasma-enhanced chemical vapor deposition device.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜装置,该装置为待处理的金属管状工件置于管型真空室内,在金属管状工件的中心轴向设置一钨丝电极,钨丝电极两端通过真空室密封法兰引出,在钨丝电极与真空室壁之间连接直流脉冲电源或射频电源,在真空室外缠绕漆包线构成电磁线圈。The device for depositing thin films on the inner surface of a long tube by plasma-enhanced chemical vapor deposition, the device is to place the metal tubular workpiece to be processed in a tubular vacuum chamber, and a tungsten wire electrode is arranged axially in the center of the metal tubular workpiece, and the tungsten wire Both ends of the electrode are led out through the sealing flange of the vacuum chamber, a DC pulse power supply or a radio frequency power supply is connected between the tungsten wire electrode and the vacuum chamber wall, and an enameled wire is wound outside the vacuum chamber to form an electromagnetic coil.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜装置,该装置包括:直流脉冲电源或射频电源、钨丝电极、管状工件、真空室、线圈转动链条传动装置、电磁线圈、进气管,具体结构如下:The device for depositing thin films on the inner surface of long tubes by plasma-enhanced chemical vapor deposition includes: DC pulse power supply or radio frequency power supply, tungsten wire electrode, tubular workpiece, vacuum chamber, coil rotating chain transmission device, electromagnetic coil, air intake pipe , the specific structure is as follows:

管状工件设置于真空室中,钨丝电极穿设于管状工件,直流脉冲电源或射频电源的正极连接钨丝电极,直流脉冲电源或射频电源的负极连接管状工件;真空室的外侧设置线圈转动链条传动装置,线圈转动链条传动装置的外侧设置电磁线圈;进气管的一端伸至管状工件中,进气管的另一端伸至真空室外侧连接气瓶。The tubular workpiece is set in the vacuum chamber, and the tungsten wire electrode is pierced through the tubular workpiece. The positive pole of the DC pulse power supply or the RF power supply is connected to the tungsten wire electrode, and the negative pole of the DC pulse power supply or the RF power supply is connected to the tubular workpiece; a coil rotation chain is set outside the vacuum chamber. Transmission device, the coil rotation chain transmission device is provided with an electromagnetic coil outside; one end of the air intake pipe extends into the tubular workpiece, and the other end of the air intake pipe extends to the outside of the vacuum chamber to connect with the gas cylinder.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜装置,真空室的内侧设置加热器。The device for depositing a thin film on the inner surface of a long tube by using plasma enhanced chemical vapor deposition, and a heater is arranged inside the vacuum chamber.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜装置,真空室的两端分别设置密封法兰。In the device for depositing thin films on the inner surface of long tubes by using plasma enhanced chemical vapor deposition, sealing flanges are respectively arranged at both ends of the vacuum chamber.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜装置,进气管上设置气体质量流量计。The device for depositing a thin film on the inner surface of a long tube by plasma-enhanced chemical vapor deposition, and a gas mass flowmeter is arranged on the inlet tube.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜装置,线圈转动链条传动装置与链条传动电机传动连接,链条传动电机与链条传动电机电源。The device for depositing thin films on the inner surface of the long tube by plasma-enhanced chemical vapor deposition, the coil rotating chain transmission device is connected to the chain transmission motor, and the chain transmission motor is connected to the chain transmission motor power supply.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜装置,管状工件为通孔或盲孔结构。In the device for depositing a thin film on the inner surface of a long tube by using plasma enhanced chemical vapor deposition, the tubular workpiece has a through-hole or blind-hole structure.

一种用等离子体增强化学气相沉积在长管内表面沉积薄膜方法,将待处理的金属管状工件置于管型真空室内,在金属管状工件的中心轴向设置一钨丝电极,电极两端通过真空室密封法兰引出,在钨丝电极与真空室壁之间连接直流脉冲电源或射频电源,不仅激励放电以产生等离子体,还在管内部建立偏压电场,对等离子体进行加速以提高膜基结合力;在真空室外缠绕漆包线构成电磁线圈,电磁线圈连接直流稳压电源以产生电磁场;利用磁场和电场对等离子体的约束和控制,从而实现等离子体在金属管状工件内壁沉积薄膜的目的。A method of depositing a film on the inner surface of a long tube by plasma-enhanced chemical vapor deposition. The metal tubular workpiece to be processed is placed in a tube-shaped vacuum chamber, and a tungsten wire electrode is arranged in the central axis of the metal tubular workpiece. Both ends of the electrode pass through the vacuum chamber. The chamber sealing flange is drawn out, and a DC pulse power supply or a radio frequency power supply is connected between the tungsten wire electrode and the vacuum chamber wall, which not only stimulates the discharge to generate plasma, but also establishes a bias electric field inside the tube to accelerate the plasma to improve the film thickness. base binding force; the enameled wire is wound outside the vacuum chamber to form an electromagnetic coil, and the electromagnetic coil is connected to a DC regulated power supply to generate an electromagnetic field; the magnetic field and electric field are used to confine and control the plasma, so as to achieve the purpose of plasma depositing a thin film on the inner wall of a metal tubular workpiece.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜方法,电磁线圈固定到一个链轮系统上,链轮系统连接一个直流电机,直流电机连接直流电源,将直流电源通电后电机转动以带动链轮系统绕自身轴线旋转,进一步实现电磁线圈与链轮系统同步旋转。In the method of depositing a thin film on the inner surface of a long tube by plasma-enhanced chemical vapor deposition, the electromagnetic coil is fixed on a sprocket system, the sprocket system is connected to a DC motor, and the DC motor is connected to a DC power supply. After the DC power supply is energized, the motor rotates to Drive the sprocket system to rotate around its own axis, and further realize the synchronous rotation of the electromagnetic coil and the sprocket system.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜方法,利用等离子体增强化学气相装置沉积薄膜,其具体过程为:将待处理的金属管状工件清洗干燥后置于管型真空室内,抽真空至真空室内真空度达到5×10-3Pa~1×10-2Pa时,通入工作气体,气压为1~100Pa,开启直流脉冲电源或射频电源激励放电以产生等离子体,对金属管状工件表面进行溅射清洗5~40分钟;同时开启加热器将真空室温度加热至所需温度300~700℃;此后在真空室内通入反应气体或者反应气体与工作气体的混合气体,混合气体中反应气体与工作气体的流量比为3~5:1,气压为1~600Pa,反应气体放电以产生等离子体;同时调节电磁线圈电流为0.5~10A,磁感应强度范围为100~3000高斯,开启直流电源,带动直流电机及链轮转动,转动速率为5~20转/分钟,镀膜时间为20~120分钟;镀膜结束后,迅速关闭直流脉冲电源或射频电源,关闭直流电源开关,停止气体通入,继续抽真空至工件随炉冷却至100℃以下,镀膜过程结束,打开真空室,取出工件。The method for depositing thin films on the inner surface of long tubes by plasma-enhanced chemical vapor deposition uses plasma-enhanced chemical vapor deposition to deposit thin films. The specific process is as follows: the metal tubular workpiece to be processed is cleaned and dried and then placed in a tubular vacuum chamber. Vacuumize until the vacuum degree in the vacuum chamber reaches 5×10 -3 Pa~1×10 -2 Pa, introduce the working gas, the pressure is 1~100Pa, turn on the DC pulse power supply or RF power supply to stimulate the discharge to generate plasma, which will damage the metal The surface of the tubular workpiece is sputtered and cleaned for 5 to 40 minutes; at the same time, the heater is turned on to heat the vacuum chamber to the required temperature of 300 to 700°C; The flow ratio of the reactive gas to the working gas is 3-5:1, the air pressure is 1-600Pa, and the reactive gas is discharged to generate plasma; at the same time, the electromagnetic coil current is adjusted to 0.5-10A, and the magnetic induction range is 100-3000 Gauss. The DC power supply drives the DC motor and the sprocket to rotate. The rotation rate is 5-20 rpm, and the coating time is 20-120 minutes. In, continue to evacuate until the workpiece cools down to below 100°C with the furnace, the coating process is over, open the vacuum chamber, and take out the workpiece.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜方法,直流脉冲电源的电压为1~100kV,频率为1~100kHz,占空比为5~85%连续可调。In the method for depositing thin films on the inner surface of long tubes by using plasma enhanced chemical vapor deposition, the voltage of the DC pulse power supply is 1-100kV, the frequency is 1-100kHz, and the duty cycle is 5-85%, which is continuously adjustable.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜方法,其特征在于,工作气体为氩气、氪气或疝气。The method for depositing a thin film on the inner surface of a long tube by plasma enhanced chemical vapor deposition is characterized in that the working gas is argon, krypton or gas.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜方法,反应气体为CH4、C2H2、H2、TiCl4、NH3、SiCl4、AlCl3、O2及H2气体中的一种或两种以上混合。In the method of depositing thin films on the inner surface of long tubes by plasma enhanced chemical vapor deposition, the reaction gases are CH 4 , C 2 H 2 , H 2 , TiCl 4 , NH 3 , SiCl 4 , AlCl 3 , O 2 and H 2 gases One or more of them are mixed.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜方法,金属管状工件是长度为20~1000mm具有管孔结构的金属模具。In the method for depositing a thin film on the inner surface of a long tube by plasma enhanced chemical vapor deposition, the metal tubular workpiece is a metal mold with a tube hole structure with a length of 20-1000 mm.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜方法,金属管状工件是直径为10~200mm、长度为20~1000mm,壁厚为1~20mm的具有管孔结构的金属长管。In the method for depositing a thin film on the inner surface of a long tube by plasma enhanced chemical vapor deposition, the metal tubular workpiece is a long metal tube with a tube hole structure with a diameter of 10-200 mm, a length of 20-1000 mm, and a wall thickness of 1-20 mm.

所述的用等离子体增强化学气相沉积在长管内表面沉积薄膜方法,金属管状工件是长度为20~1000mm的具有管孔结构的金属零件。In the method for depositing a thin film on the inner surface of a long tube by plasma enhanced chemical vapor deposition, the metal tubular workpiece is a metal part with a tube hole structure and a length of 20-1000 mm.

本实用新型的核心思想是:为了有效改善等离子体的利用效率,提高在管内部等离子体的轴向均匀性及薄膜沉积效率,在管内放电产生等离子体后,利用电磁线圈产生的磁场与等离子体的交互作用,对等离子体束流进行约束控制,同时用电机驱动一个链轮系统来控制电磁线圈绕中心轴向旋转,从而在很大程度上保证管腔内壁薄膜沉积的均匀性。此外,为了加强离子与内壁的良好结合,在管腔内部设置脉冲电场,在管壁施加脉冲负偏压对正离子进行加速,以保证薄膜与管内壁的良好结合。The core idea of the utility model is: in order to effectively improve the utilization efficiency of the plasma, improve the axial uniformity of the plasma inside the tube and the film deposition efficiency, after the plasma is generated by the discharge in the tube, the magnetic field generated by the electromagnetic coil and the plasma The interaction of the plasma beam is restricted and controlled, and a sprocket system is driven by a motor to control the rotation of the electromagnetic coil around the central axis, thereby ensuring the uniformity of the film deposition on the inner wall of the lumen to a large extent. In addition, in order to strengthen the good combination of ions and the inner wall, a pulsed electric field is set inside the lumen, and a pulsed negative bias is applied to the tube wall to accelerate the positive ions to ensure a good combination of the film and the inner wall of the tube.

本实用新型的有益效果是:The beneficial effects of the utility model are:

1、本实用新型采用磁场对等离子体束在管内的扩散进行聚焦和约束,在很大程度上保证了等离子体束流的利用效率。1. The utility model uses a magnetic field to focus and restrain the diffusion of the plasma beam in the tube, which largely ensures the utilization efficiency of the plasma beam.

2、本实用新型采用电磁线圈产生的电磁场来约束等离子体,通过调整电磁线圈的电流大小来调整磁感应强度,参数可调方便,使得电磁场对等离子体束流的聚焦和约束变得容易控制。2. The utility model uses the electromagnetic field generated by the electromagnetic coil to constrain the plasma, and adjusts the magnetic induction intensity by adjusting the current of the electromagnetic coil. The parameters are adjustable and convenient, making it easy to control the focusing and restraint of the plasma beam by the electromagnetic field.

3、本实用新型将直流脉冲电源施加到管状工件上,在管内形成脉冲负偏压电场,对正离子进行加速,以保证薄膜与管内壁的良好结合。3. The utility model applies a DC pulse power supply to the tubular workpiece, forms a pulsed negative bias electric field in the tube, and accelerates the positive ions to ensure a good combination of the film and the inner wall of the tube.

4、本实用新型采用了管与电磁线圈之间的一个相对旋转,用电机驱动一个链轮系统来控制电磁线圈绕中心轴向旋转,进一步提高管内薄膜轴向的均匀性。4. The utility model adopts a relative rotation between the tube and the electromagnetic coil, and uses a motor to drive a sprocket system to control the axial rotation of the electromagnetic coil around the center, further improving the axial uniformity of the film in the tube.

5、本实用新型解决了PECVD在长管内壁镀膜不均匀的技术难题,采用磁场和电场与等离子体交互作用,有效提高了在管状工件内壁镀膜的均匀性和沉积质量,与常规的镀膜工艺相比,管内薄膜轴向均匀性提高到80%以上,尤其适用于以内壁作为服役表面的管状工件的内表面镀膜,有效提高其使用寿命。5. The utility model solves the technical problem of uneven PECVD coating on the inner wall of long tubes, and uses the interaction of magnetic field and electric field with plasma to effectively improve the uniformity and deposition quality of the coating on the inner wall of tubular workpieces. Compared with the conventional coating process Ratio, the axial uniformity of the film in the tube is increased to more than 80%, especially suitable for the inner surface coating of the tubular workpiece with the inner wall as the service surface, effectively improving its service life.

附图说明Description of drawings

图1是本实用新型的采用磁场增强的PECVD装置及管状工件相对位置摆放示意图,其中管状工件为通孔结构。FIG. 1 is a schematic diagram of relative positions of a PECVD device using magnetic field enhancement and a tubular workpiece according to the present invention, wherein the tubular workpiece has a through-hole structure.

图2是本实用新型的采用磁场增强的PECVD装置及管状工件相对位置摆放示意图,其中管状工件为盲孔结构。Fig. 2 is a schematic diagram of relative positions of a PECVD device using magnetic field enhancement and a tubular workpiece according to the present invention, wherein the tubular workpiece has a blind hole structure.

图中,1直流脉冲电源或射频电源;2钨丝电极;3管状工件;4真空室;5加热器;6线圈转动链条传动装置;7电磁线圈;8密封法兰;9进气管;10气体质量流量计;11气瓶;12链条传动电机;13链条传动电机电源。In the figure, 1 DC pulse power supply or radio frequency power supply; 2 tungsten wire electrode; 3 tubular workpiece; 4 vacuum chamber; 5 heater; 6 coil rotating chain transmission device; 7 electromagnetic coil; Mass flow meter; 11 cylinders; 12 chain drive motor; 13 chain drive motor power supply.

具体实施方式:Detailed ways:

如图1-图2所示,本实用新型的采用磁场增强的PECVD装置主要包括:直流脉冲电源或射频电源1、钨丝电极2、管状工件3、真空室4、加热器5、线圈转动链条传动装置6、电磁线圈7、密封法兰8、进气管9、气体质量流量计10、气瓶11、链条传动电机12、链条传动电机电源13等,具体结构如下:As shown in Fig. 1-Fig. 2, the PECVD device adopting magnetic field enhancement of the utility model mainly includes: DC pulse power supply or radio frequency power supply 1, tungsten wire electrode 2, tubular workpiece 3, vacuum chamber 4, heater 5, coil rotating chain Transmission device 6, electromagnetic coil 7, sealing flange 8, intake pipe 9, gas mass flow meter 10, gas cylinder 11, chain drive motor 12, chain drive motor power supply 13, etc. The specific structure is as follows:

管状工件3设置于真空室4中,钨丝电极2穿设于管状工件3,直流脉冲电源或射频电源1的正极连接钨丝电极2,直流脉冲电源或射频电源1的负极连接管状工件3;真空室4的内侧设置加热器5,真空室4的外侧设置线圈转动链条传动装置6,线圈转动链条传动装置6的外侧设置电磁线圈7,真空室4的两端分别设置密封法兰8,进气管9的一端伸至管状工件3中,进气管9的另一端伸至真空室4外侧连接气瓶11,进气管9上设置气体质量流量计10;线圈转动链条传动装置6与链条传动电机12传动连接,链条传动电机12与链条传动电机电源13。本实用新型中,管状工件3为通孔或盲孔结构。The tubular workpiece 3 is set in the vacuum chamber 4, the tungsten wire electrode 2 is pierced through the tubular workpiece 3, the positive pole of the DC pulse power supply or the radio frequency power supply 1 is connected to the tungsten wire electrode 2, and the negative pole of the DC pulse power supply or the radio frequency power supply 1 is connected to the tubular workpiece 3; The inner side of the vacuum chamber 4 is provided with a heater 5, the outer side of the vacuum chamber 4 is provided with a coil rotating chain transmission device 6, the outer side of the coil rotating chain transmission device 6 is provided with an electromagnetic coil 7, and the two ends of the vacuum chamber 4 are respectively provided with sealing flanges 8 for further One end of the gas pipe 9 extends into the tubular workpiece 3, the other end of the air inlet pipe 9 extends to the outside of the vacuum chamber 4 to connect to the gas cylinder 11, and the gas mass flow meter 10 is arranged on the air inlet pipe 9; the coil rotation chain transmission device 6 and the chain transmission motor 12 Transmission connection, chain drive motor 12 and chain drive motor power supply 13. In the utility model, the tubular workpiece 3 is a through hole or blind hole structure.

将待处理的金属管状工件3置于管型真空室4内,在金属管状工件3的中心轴向设置一钨丝电极2,钨丝电极2两端通过真空室密封法兰8引出,在钨丝电极2与真空室4壁之间连接直流脉冲电源或射频电源1,不仅可激励放电以产生等离子体,还可在管内部建立偏压电场,对等离子体进行加速以提高膜基结合力;在真空室4外缠绕漆包线构成电磁线圈7,电磁线圈7连接直流稳压电源以产生电磁场;利用磁场和电场对等离子体的约束和控制,从而实现等离子体在金属管状工件3内壁沉积薄膜的目的。所述电磁线圈7固定到一个链轮系统(线圈转动链条传动装置6)上,链轮系统连接一个直流电机(链条传动电机12),直流电机连接直流电源(链条传动电机电源13),将直流电源通电后电机转动以带动链轮系统绕自身轴线旋转,进一步实现电磁线圈与链轮系统同步旋转。The metal tubular workpiece 3 to be processed is placed in the tubular vacuum chamber 4, and a tungsten wire electrode 2 is arranged axially in the center of the metal tubular workpiece 3. The two ends of the tungsten wire electrode 2 are drawn out through the vacuum chamber sealing flange 8, and the A DC pulse power supply or RF power supply 1 is connected between the wire electrode 2 and the wall of the vacuum chamber 4, which can not only stimulate the discharge to generate plasma, but also establish a bias electric field inside the tube to accelerate the plasma to improve the bonding force of the film base The enameled wire is wound outside the vacuum chamber 4 to form an electromagnetic coil 7, and the electromagnetic coil 7 is connected to a DC stabilized power supply to generate an electromagnetic field; the plasma is restrained and controlled by the magnetic field and the electric field, so as to realize the deposition of a thin film on the inner wall of the metal tubular workpiece 3 by the plasma Purpose. The electromagnetic coil 7 is fixed to a sprocket system (coil rotating chain drive 6), the sprocket system is connected to a DC motor (chain drive motor 12), the DC motor is connected to a DC power supply (chain drive motor power supply 13), and the DC After the power is turned on, the motor rotates to drive the sprocket system to rotate around its own axis, further realizing the synchronous rotation of the electromagnetic coil and the sprocket system.

本实用新型是通过在等离子体化学气相沉积薄膜过程中,利用磁场对等离子体进行约束和控制,利用电场对等离子体实现加速定向流动,从而在很大程度上保证管腔内壁薄膜沉积的均匀性和膜基结合力,从而实现等离子体在金属管状工件内表面均匀沉积薄膜的目的。The utility model utilizes the magnetic field to constrain and control the plasma during the plasma chemical vapor deposition film process, and utilizes the electric field to accelerate the directional flow of the plasma, thereby ensuring the uniformity of the film deposition on the inner wall of the tube cavity to a large extent. The bonding force with the film base, so as to achieve the purpose of uniformly depositing a thin film on the inner surface of the metal tubular workpiece by plasma.

将待处理的金属管状工件3清洗干燥后置于管型真空室4内,抽真空至真空室4内真空度达到5×10-3Pa~1×10-2Pa时,通入工作气体,气压为1~100Pa,开启脉冲或射频电源激励放电以产生等离子体,对金属管状工件4表面进行溅射清洗5~40分钟。同时,开启加热器5将真空室4温度加热至所需温度(300~700℃);此后在真空室4内通入反应气体或者反应气体与工作气体的混合气体(混合气体中反应气体与工作气体的流量比为3~5:1),气压为1~600Pa,反应气体放电以产生等离子体。同时调节电磁线圈电流为0.5~10A,磁感应强度范围为100~3000高斯,开启直流电源(链条传动电机电源13),带动直流电机(链条传动电机12)及链轮(线圈转动链条传动装置6)转动,转动速率为5~20转/分钟,镀膜时间为20~120分钟;镀膜结束后,迅速关闭脉冲或射频电源,关闭直流电源开关,停止气体通入,继续抽真空至工件随炉冷却至100℃以下,镀膜过程结束,打开真空室,取出工件。After cleaning and drying the metal tubular workpiece 3 to be processed, place it in the tubular vacuum chamber 4, and pump the vacuum until the vacuum degree in the vacuum chamber 4 reaches 5×10 -3 Pa~1×10 -2 Pa, and then inject the working gas, The air pressure is 1-100 Pa, the pulse or radio frequency power supply is turned on to stimulate the discharge to generate plasma, and the surface of the metal tubular workpiece 4 is sputtered and cleaned for 5-40 minutes. At the same time, turn on the heater 5 to heat the temperature of the vacuum chamber 4 to the required temperature (300-700°C); after that, the reaction gas or the mixed gas of the reaction gas and the working gas (the reaction gas and the working gas in the mixed gas) are introduced into the vacuum chamber 4 The gas flow ratio is 3-5:1), the pressure is 1-600Pa, and the reactive gas is discharged to generate plasma. At the same time, adjust the electromagnetic coil current to 0.5-10A, and the magnetic induction range is 100-3000 gauss, turn on the DC power supply (chain drive motor power supply 13), and drive the DC motor (chain drive motor 12) and sprocket (coil rotation chain drive device 6) Rotate, the rotation rate is 5-20 rpm, and the coating time is 20-120 minutes; after the coating is completed, quickly turn off the pulse or radio frequency power supply, turn off the DC power switch, stop the gas supply, and continue to vacuum until the workpiece cools down with the furnace. Below 100°C, the coating process is over, open the vacuum chamber, and take out the workpiece.

本实用新型中,放置于管型真空室的磁场发生装置为一个电磁线圈,线径0.3~2.5mm,缠绕密度为10~100匝/mm,电磁线圈用支撑筒支撑,支撑筒外径为200~500mm,长度为200~2000mm,通过调节电磁线圈电流的大小来调节磁场强度的大小。In the utility model, the magnetic field generating device placed in the tubular vacuum chamber is an electromagnetic coil with a wire diameter of 0.3-2.5 mm and a winding density of 10-100 turns/mm. The electromagnetic coil is supported by a support cylinder whose outer diameter is 200 ~500mm, the length is 200~2000mm, the magnetic field strength can be adjusted by adjusting the current of the electromagnetic coil.

本实用新型中,直流脉冲电源的电压为1~100kV,频率为1~100kHz,占空比为5~85%连续可调。In the utility model, the voltage of the DC pulse power supply is 1-100kV, the frequency is 1-100kHz, and the duty ratio is 5-85%, which is continuously adjustable.

本实用新型中,金属管状工件是长度为20~1000mm具有管孔结构的金属模具。In the utility model, the metal tubular workpiece is a metal mold with a length of 20-1000 mm and a tube hole structure.

本实用新型中,金属管状工件是直径为10~200mm、长度为20~1000mm,壁厚为1~20mm的具有管孔结构的金属长管。In the utility model, the metal tubular workpiece is a long metal tube with a tube hole structure with a diameter of 10-200mm, a length of 20-1000mm, and a wall thickness of 1-20mm.

本实用新型中,金属管状工件是长度为20~1000mm的具有管孔结构的金属零件。In the utility model, the metal tubular workpiece is a metal part with a tube hole structure and a length of 20-1000 mm.

实施例1Example 1

将内径为Φ50mm、壁厚为5mm、长度为300mm具有通孔的不锈钢长管清洗、烘干后,放置在管型真空室内,如图1所示,抽真空至真空室内真空度达到7×10-3Pa时,通入氩气,气压为20Pa,开启直流脉冲电源激励放电以产生等离子体,对金属管状工件表面进行溅射清洗20分钟。同时开启加热器将真空室温度加热至温度为300℃;此后在真空室内通入乙炔气,调制乙炔气体与氩气流量比为5:1,且将气压调制为5.0Pa,开启直流脉冲电源以激励反应气体放电以产生等离子体。同时调节电磁线圈电流为2A,磁感应强度范围为1200高斯,开启直流电源,带动直流电机及链轮转动,转动速率为5转/分钟,镀膜时间为30分钟;镀膜结束后,迅速关闭直流脉冲电源,关闭直流电源开关,停止气体通入,继续抽真空至工件随炉冷却至100℃以下,镀膜过程结束,打开真空室,取出工件。本实施例中,直流脉冲电源的电压为50kV,频率为50kHz,占空比为40%。Clean and dry a long stainless steel tube with an inner diameter of Φ50mm, a wall thickness of 5mm, and a length of 300mm with a through hole, and place it in a tube-shaped vacuum chamber, as shown in Figure 1, and evacuate until the vacuum degree in the vacuum chamber reaches 7×10 At -3 Pa, argon gas is introduced, the pressure is 20 Pa, the DC pulse power supply is turned on to stimulate the discharge to generate plasma, and the surface of the metal tubular workpiece is sputtered and cleaned for 20 minutes. At the same time, turn on the heater to heat the temperature of the vacuum chamber to 300°C; after that, introduce acetylene gas into the vacuum chamber, adjust the flow ratio of acetylene gas to argon gas to 5:1, adjust the air pressure to 5.0Pa, and turn on the DC pulse power supply to The reactant gas is excited to discharge to generate a plasma. At the same time, adjust the current of the electromagnetic coil to 2A, the range of magnetic induction intensity to 1200 gauss, turn on the DC power supply, drive the DC motor and the sprocket to rotate, the rotation rate is 5 rpm, and the coating time is 30 minutes; after the coating is completed, quickly turn off the DC pulse power supply , turn off the DC power switch, stop the gas supply, continue vacuuming until the workpiece cools down to below 100°C with the furnace, the coating process is over, open the vacuum chamber, and take out the workpiece. In this embodiment, the voltage of the DC pulse power supply is 50kV, the frequency is 50kHz, and the duty cycle is 40%.

本实施方式可以在不锈钢管内径为Φ50mm的内表面沉积类金刚石(DLC)膜,薄膜均匀致密,DLC薄膜的厚度为0.5~2μm,薄膜显微硬度达到18GPa以上,能显著提高不锈钢管内壁的耐磨性能,进而提高不锈钢管的使用寿命。In this embodiment, a diamond-like carbon (DLC) film can be deposited on the inner surface of the stainless steel tube with an inner diameter of Φ50mm. The film is uniform and dense. Grinding performance, thereby improving the service life of stainless steel pipes.

实施例2Example 2

将Φ50×80mm的具有Φ25×60mm盲孔的不锈钢管清洗、烘干后,放置在管型真空室内,如图2所示,与图1不同的是,待处理的不锈钢管具有盲孔结构。抽真空至真空室内真空度达到6×10-3Pa时,通入氩气,气压为10Pa,开启直流脉冲电源激励放电以产生等离子体,对金属管状工件表面进行溅射清洗30分钟。同时开启加热器将真空室温度加热至温度为350℃;此后在真空室内通入乙炔气,调制乙炔气体与氩气流量比为4:1,且将气压调制为4.0Pa,开启直流脉冲电源以激励反应气体放电以产生等离子体。同时调节电磁线圈电流为3A,磁感应强度范围为1800高斯,开启直流电源,带动直流电机及链轮转动,转动速率为5转/分钟,镀膜时间为120分钟;镀膜结束后,迅速关闭直流脉冲电源,关闭直流电源开关,停止气体通入,继续抽真空至工件随炉冷却至100℃以下,镀膜过程结束,打开真空室,取出工件。本实施例中,直流脉冲电源的电压为10kV,频率为60kHz,占空比为30%。Clean and dry a Φ50×80mm stainless steel tube with a Φ25×60mm blind hole, and place it in a tubular vacuum chamber, as shown in Figure 2. Unlike Figure 1, the stainless steel tube to be treated has a blind hole structure. After evacuating until the vacuum degree in the vacuum chamber reaches 6×10 -3 Pa, introduce argon gas at a pressure of 10 Pa, turn on the DC pulse power supply to stimulate the discharge to generate plasma, and perform sputter cleaning on the surface of the metal tubular workpiece for 30 minutes. At the same time, turn on the heater to heat the temperature of the vacuum chamber to 350°C; after that, introduce acetylene gas into the vacuum chamber, adjust the flow ratio of acetylene gas to argon gas to 4:1, adjust the air pressure to 4.0Pa, and turn on the DC pulse power supply to The reactant gas is excited to discharge to generate a plasma. At the same time, adjust the current of the electromagnetic coil to 3A, the range of magnetic induction intensity to 1800 Gauss, turn on the DC power supply, drive the DC motor and the sprocket to rotate, the rotation rate is 5 rpm, and the coating time is 120 minutes; after the coating is completed, quickly turn off the DC pulse power supply , turn off the DC power switch, stop the gas supply, continue vacuuming until the workpiece cools down to below 100°C with the furnace, the coating process is over, open the vacuum chamber, and take out the workpiece. In this embodiment, the voltage of the DC pulse power supply is 10kV, the frequency is 60kHz, and the duty cycle is 30%.

本实施方式可以在不锈钢管内径为Φ25mm的内表面沉积类金刚石(DLC)膜,薄膜均匀致密,DLC薄膜的厚度为0.5~2μm,薄膜显微硬度达到16GPa以上,能显著提高不锈钢管内壁的耐磨性能,进而提高不锈钢管的使用寿命。In this embodiment, a diamond-like carbon (DLC) film can be deposited on the inner surface of the stainless steel tube with an inner diameter of Φ25mm. The film is uniform and dense. Grinding performance, thereby improving the service life of stainless steel pipes.

实施例3Example 3

将Φ50×200mm的具有Φ40×200mm通孔的低碳钢零件清洗、烘干后,放置在管型真空室内,如图1所示,抽真空至真空室内真空度达到5×10-3Pa时,通入氩气,气压为8Pa,开启直流脉冲电源激励放电以产生等离子体,对金属管状工件表面进行溅射清洗10分钟。同时开启加热器将真空室温度加热至温度为400℃;此后在真空室内通入TiCl4与NH3混合气体,气体比例为1:1,且将气压调制为200Pa,开启直流脉冲电源以激励反应气体放电以产生等离子体。同时调节电磁线圈电流为2A,磁感应强度范围为1200高斯,开启直流电源,带动直流电机及链轮转动,转动速率为10转/分钟,镀膜时间为60分钟;镀膜结束后,迅速关闭直流脉冲电源,关闭直流电源开关,停止气体通入,继续抽真空至工件随炉冷却至100℃以下,镀膜过程结束,打开真空室,取出工件。本实施例中,直流脉冲电源的电压为20kV,频率为20kHz,占空比为30%。After cleaning and drying the Φ50×200mm low-carbon steel parts with Φ40×200mm through holes, place them in a tubular vacuum chamber, as shown in Figure 1, and evacuate until the vacuum degree in the vacuum chamber reaches 5×10 -3 Pa , into the argon gas, the pressure is 8Pa, turn on the DC pulse power supply to stimulate the discharge to generate plasma, and perform sputter cleaning on the surface of the metal tubular workpiece for 10 minutes. At the same time, turn on the heater to heat the temperature of the vacuum chamber to 400°C; after that, a mixed gas of TiCl 4 and NH 3 is introduced into the vacuum chamber, the gas ratio is 1:1, and the air pressure is adjusted to 200Pa, and the DC pulse power supply is turned on to stimulate the reaction The gas is discharged to create a plasma. At the same time, adjust the electromagnetic coil current to 2A, the magnetic induction intensity range to 1200 Gauss, turn on the DC power supply, drive the DC motor and the sprocket to rotate, the rotation rate is 10 rpm, and the coating time is 60 minutes; after the coating is completed, quickly turn off the DC pulse power supply , turn off the DC power switch, stop the gas supply, continue vacuuming until the workpiece cools down to below 100°C with the furnace, the coating process is over, open the vacuum chamber, and take out the workpiece. In this embodiment, the voltage of the DC pulse power supply is 20kV, the frequency is 20kHz, and the duty cycle is 30%.

本实施方式可以在低碳钢零件内径为Φ40mm的内表面沉积氮化钛(TiN)薄膜,薄膜均匀致密,TiN薄膜的厚度为2μm,薄膜显微硬度达到21GPa以上,能显著提高低碳钢零件内壁的耐磨及耐腐蚀性能,进而提高低碳钢零件的使用寿命。This embodiment can deposit a titanium nitride (TiN) film on the inner surface of a low-carbon steel part with an inner diameter of Φ40mm. The film is uniform and dense. The wear resistance and corrosion resistance of the inner wall can improve the service life of low carbon steel parts.

实施例4Example 4

将Φ50×200mm的具有Φ30×150mm通孔的硬质合金零件清洗、烘干后,放置在管型真空室内,如图1所示,抽真空至真空室内真空度达到6×10-3Pa时,通入氩气,气压为20Pa,开启直流脉冲电源激励放电以产生等离子体,对金属管状工件表面进行溅射清洗20分钟。同时开启加热器将真空室温度加热至温度为300℃;此后在真空室内通入AlCl3、O2及H2的混合气体,气体比例为2:3:3,气压为100Pa,开启直流脉冲电源以激励反应气体放电以产生等离子体。同时调节电磁线圈电流为2A,磁感应强度范围为1200高斯,开启直流电源,带动直流电机及链轮转动,转动速率为5转/分钟,镀膜时间为60分钟;镀膜结束后,迅速关闭直流脉冲电源,关闭直流电源开关,停止气体通入,继续抽真空至工件随炉冷却至100℃以下,镀膜过程结束,打开真空室,取出工件。本实施例中,直流脉冲电源的电压为40kV,频率为80kHz,占空比为60%。Clean and dry a Φ50×200mm hard alloy part with a Φ30×150mm through hole, then place it in a tubular vacuum chamber, as shown in Figure 1, and evacuate until the vacuum degree in the vacuum chamber reaches 6×10 -3 Pa , into the argon gas, the pressure is 20Pa, turn on the DC pulse power supply to stimulate the discharge to generate plasma, and perform sputter cleaning on the surface of the metal tubular workpiece for 20 minutes. At the same time, turn on the heater to heat the temperature of the vacuum chamber to 300°C; after that, pass the mixed gas of AlCl 3 , O 2 and H 2 into the vacuum chamber, the gas ratio is 2:3:3, the air pressure is 100Pa, and the DC pulse power supply is turned on To excite the reactive gas discharge to generate plasma. At the same time, adjust the current of the electromagnetic coil to 2A, the range of magnetic induction to 1200 gauss, turn on the DC power supply, drive the DC motor and the sprocket to rotate, the rotation rate is 5 rpm, and the coating time is 60 minutes; after the coating is completed, quickly turn off the DC pulse power supply , turn off the DC power switch, stop the gas supply, continue vacuuming until the workpiece cools down to below 100°C with the furnace, the coating process is over, open the vacuum chamber, and take out the workpiece. In this embodiment, the voltage of the DC pulse power supply is 40kV, the frequency is 80kHz, and the duty cycle is 60%.

本实施方式可以在硬质合金零件内径为Φ30mm的内表面沉积氧化铝(Al2O3)膜,薄膜均匀致密,氧化铝薄膜的厚度为1.8μm,薄膜显微硬度达到20GPa以上,能显著提高硬质合金零件内壁的耐磨性能,进而提高不锈钢管的使用寿命。In this embodiment, the aluminum oxide (Al 2 O 3 ) film can be deposited on the inner surface of the hard alloy part with an inner diameter of Φ30mm. The film is uniform and dense. The wear resistance of the inner wall of the cemented carbide parts can improve the service life of the stainless steel pipe.

Claims (7)

  1. One kind with plasma enhanced chemical vapor deposition at long tube internal surface thin film deposition device, it is characterized in that, this device is placed in cast vacuum chamber for pending tubular metal workpiece, at the central shaft of tubular metal workpiece to a tungsten filament electrode is set, draw by vacuum chamber tongued and grooved flanges at tungsten filament electrode two ends, between tungsten filament electrode and vacuum-chamber wall, be connected direct current pulse power source or radio-frequency power supply, at vacuum chamber, be wound around enameled wire outward and form solenoid.
  2. 2. the plasma enhanced chemical vapor deposition of using according to claim 1 is at long tube internal surface thin film deposition device, it is characterized in that, this device comprises: direct current pulse power source or radio-frequency power supply, tungsten filament electrode, tubular workpiece, vacuum chamber, coil rotating link chain transmission mechanism, solenoid, inlet pipe, and concrete structure is as follows:
    Tubular workpiece is arranged in vacuum chamber, and tungsten filament electrode is arranged in tubular workpiece, and the positive pole of direct current pulse power source or radio-frequency power supply connects tungsten filament electrode, the negative pole connecting tubular workpiece of direct current pulse power source or radio-frequency power supply; The arranged outside coil rotating link chain transmission mechanism of vacuum chamber, the arranged outside solenoid of coil rotating link chain transmission mechanism; One end of inlet pipe extends in tubular workpiece, and the other end of inlet pipe extends vacuum chamber outside and connects gas cylinder.
  3. 3. the plasma enhanced chemical vapor deposition of using according to claim 2, at long tube internal surface thin film deposition device, is characterized in that, the inner side of vacuum chamber arranges well heater.
  4. 4. the plasma enhanced chemical vapor deposition of using according to claim 2, at long tube internal surface thin film deposition device, is characterized in that, the two ends of vacuum chamber arrange respectively tongued and grooved flanges.
  5. 5. the plasma enhanced chemical vapor deposition of using according to claim 2, at long tube internal surface thin film deposition device, is characterized in that, mass-flow gas meter is set in inlet pipe.
  6. 6. the plasma enhanced chemical vapor deposition of using according to claim 2, at long tube internal surface thin film deposition device, is characterized in that, coil rotating link chain transmission mechanism is connected with chain gear motor-driven, chain gear motor and chain gear motor power.
  7. 7. the plasma enhanced chemical vapor deposition of using according to claim 2, at long tube internal surface thin film deposition device, is characterized in that, tubular workpiece is through hole or blind hole structure.
CN201320467293.5U 2013-07-31 2013-07-31 Device for depositing film on internal surface of long pipe by using plasma enhanced chemical vapor deposition Expired - Fee Related CN203498467U (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106367735A (en) * 2016-11-14 2017-02-01 张宇顺 Chemical vapor deposition device and deposition method thereof
CN108699703A (en) * 2018-04-24 2018-10-23 深圳大学 Apparatus and method for preparing surface strengthening coating
CN109338333A (en) * 2018-11-30 2019-02-15 湖南红太阳光电科技有限公司 A kind of tubular type LPCVD vacuum reaction chamber
CN111809153A (en) * 2020-06-18 2020-10-23 中国科学院高能物理研究所 Slit coating device
CN113136562A (en) * 2021-04-19 2021-07-20 东北大学 High-hardness TiN protective coating capable of being coated on deep-hole part and preparation method thereof
CN113278915A (en) * 2021-07-22 2021-08-20 艾瑞森表面技术(苏州)股份有限公司 DLC composite film with porous structure running-in layer and preparation process thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106367735A (en) * 2016-11-14 2017-02-01 张宇顺 Chemical vapor deposition device and deposition method thereof
CN106367735B (en) * 2016-11-14 2019-06-18 张宇顺 Chemical vapor deposition device and deposition method thereof
CN108699703A (en) * 2018-04-24 2018-10-23 深圳大学 Apparatus and method for preparing surface strengthening coating
CN109338333A (en) * 2018-11-30 2019-02-15 湖南红太阳光电科技有限公司 A kind of tubular type LPCVD vacuum reaction chamber
CN111809153A (en) * 2020-06-18 2020-10-23 中国科学院高能物理研究所 Slit coating device
CN111809153B (en) * 2020-06-18 2024-04-02 中国科学院高能物理研究所 Slit coating device
CN113136562A (en) * 2021-04-19 2021-07-20 东北大学 High-hardness TiN protective coating capable of being coated on deep-hole part and preparation method thereof
CN113278915A (en) * 2021-07-22 2021-08-20 艾瑞森表面技术(苏州)股份有限公司 DLC composite film with porous structure running-in layer and preparation process thereof

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