中频磁控溅射以及ECR-CVD制备DLC薄膜的新工艺研究

发布时间：2018-03-08 01:29

本文选题：DLC薄膜　切入点：磁控溅射　出处：《深圳大学》2017年硕士论文　论文类型：学位论文

【摘要】：本论文主要研究采用ECR-650复合镀膜设备制备硬质类金刚石碳膜(DLC)涂层的工艺,并对DLC涂层的性能进行了表征。通过采用电子回旋共振微波等离子体气相沉积(ECR-CVD),中频磁控溅射方法分别在单晶硅片上沉积了DLC薄膜。CVD方法中利用C2H2作为DLC薄膜的碳源,氩气为工作气体;中频磁控溅射利用高纯石墨靶材作为碳源,氩气作为工作气体,经过一系列复杂的物理或者化学过程,最终在单晶硅片基底上形成了DLC薄膜,并对其进行了表面形貌分析,计算了磁控溅射法和ECR-CVD法制备DLC薄膜时的沉积速率,分析了薄膜的结构特征,并且测试了薄膜的硬度,弹性模量和薄膜与基底之间的结合力。研究了退火对DLC薄膜性能的影响。采用中频磁控溅射时引入了强磁阴极石墨靶,与普通阴极相比引入的磁性更强,可以约束更多的电子去轰击石墨靶材从而提高离化率和增强碳离子的溅射能量,增大了薄膜的沉积速率。系统地研究了溅射电流,氩气流量和负偏压对于薄膜性能的影响。得出了溅射电流为0.85 A,氩气流量为20 sccm,负偏压为50 V时制备的DLC薄膜的硬度性能最好,测出了硬度值为17.8 GPa,此时的薄膜与基底之间的结合力为18.48 mN。ECR-CVD引入了尖端放电原理制备DLC薄膜,目的是为了增大等离子体密度及试验一些极端实验条件对DLC薄膜成膜性能的影响。与普通方式下的ECR-CVD制备的DLC薄膜相比,整体的DLC薄膜的硬度性能更好。用ECR-CVD方法制备的DLC薄膜硬度可到达30 GPa左右,硬度值最高的为30.84 GPa,并且薄膜与基底之间的结合力为103.93 mN。所以得出ECR-CVD法制备DLC薄膜的硬度性能和薄膜与基底之间的结合力性能远好于磁控溅射法制备的DLC薄膜的硬度性能与薄膜基底之间的结合力。在工业应用中,ECR-CVD法制备的DLC薄膜的硬度性能已经可以达到作为硬质涂层的硬度要求。退火处理使得DLC薄膜的表面产生一些裂纹,可能与退火温度的选择有关。退火温度达到一定温度的时候会有晶粒析出并且会产生脱落现象。DLC薄膜的SP3含量是随着退火温度的升高而减少的,因而导致DLC薄膜的硬度值与弹性模量都也随着退火温度的升高而减小。薄膜与基底之间的结合力在退火温度为200°C时会有所增强,当退火温度更高时,薄膜与基底之间的结合力则会减弱。
[Abstract]:In this paper, the process of preparing hard diamond-like carbon film (DLC) coating with ECR-650 composite coating equipment was studied. The properties of DLC coatings were characterized by electron cyclotron resonance microwave plasma vapor deposition (ECR-CVDN), and DLC thin films were deposited on single crystal silicon substrates by intermediate frequency magnetron sputtering. C _ 2H _ 2 was used as the carbon source of DLC films. Argon is the working gas, and if magnetron sputtering uses high purity graphite target as carbon source, argon as working gas, and after a series of complicated physical or chemical processes, DLC thin films are formed on single crystal silicon substrates. The surface morphology was analyzed, the deposition rate of DLC thin films was calculated by magnetron sputtering and ECR-CVD method, the structural characteristics of the films were analyzed, and the hardness of the films was tested. The influence of annealing on the properties of DLC thin films was studied. The graphite target with strong magnetic cathode was introduced in the medium frequency magnetron sputtering, and the magnetic properties of the films were stronger than those of the conventional cathode. It can restrain more electrons to bombard graphite targets, thus increasing ionization rate and sputtering energy of carbon ions, thus increasing the deposition rate of the films. The sputtering current is systematically studied. The effects of argon flow rate and negative bias voltage on the properties of the DLC films were obtained. The results showed that the best hardness properties of the DLC films were obtained when the sputtering current was 0.85 A, the argon flow rate was 20 sccm, and the negative bias voltage was 50 V. The hardness was 17.8GPa.The bonding force between the film and the substrate was 18.48 mN.ECR-CVD. The tip discharge principle was introduced to fabricate the DLC film. The aim is to increase the plasma density and to test the effect of some extreme experimental conditions on the film-forming properties of DLC thin films. The hardness of the whole DLC film is better. The hardness of the DLC film prepared by ECR-CVD method can reach about 30 GPa. The highest hardness value was 30.84 GPA, and the binding force between the film and the substrate was 103.93 mn. It was concluded that the hardness properties of DLC thin films prepared by ECR-CVD and the adhesion properties between DLC films and substrates were much better than those of DLC films prepared by magnetron sputtering. The hardness properties of DLC films prepared by ECR-CVD in industrial application can meet the hardness requirements of hard coatings. Some cracks occur on the surface of DLC films after annealing. It may be related to the selection of annealing temperature. When the annealing temperature reaches a certain temperature, there will be grain precipitation and shedding phenomenon. The SP3 content of DLC film decreases with the increase of annealing temperature. As a result, the hardness and elastic modulus of DLC thin films decrease with the increase of annealing temperature, and the adhesion between the films and the substrate increases at 200 掳C, and when the annealing temperature is higher, the adhesion between the films and the substrate increases. The adhesion between the film and the substrate will be weakened.
【学位授予单位】：深圳大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TB383.2

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