中頻磁控濺射以及ECR-CVD制備DLC薄膜的新工藝研究
本文選題:DLC薄膜 切入點(diǎn):磁控濺射 出處:《深圳大學(xué)》2017年碩士論文 論文類型:學(xué)位論文
【摘要】:本論文主要研究采用ECR-650復(fù)合鍍膜設(shè)備制備硬質(zhì)類金剛石碳膜(DLC)涂層的工藝,并對(duì)DLC涂層的性能進(jìn)行了表征。通過(guò)采用電子回旋共振微波等離子體氣相沉積(ECR-CVD),中頻磁控濺射方法分別在單晶硅片上沉積了DLC薄膜。CVD方法中利用C2H2作為DLC薄膜的碳源,氬氣為工作氣體;中頻磁控濺射利用高純石墨靶材作為碳源,氬氣作為工作氣體,經(jīng)過(guò)一系列復(fù)雜的物理或者化學(xué)過(guò)程,最終在單晶硅片基底上形成了DLC薄膜,并對(duì)其進(jìn)行了表面形貌分析,計(jì)算了磁控濺射法和ECR-CVD法制備DLC薄膜時(shí)的沉積速率,分析了薄膜的結(jié)構(gòu)特征,并且測(cè)試了薄膜的硬度,彈性模量和薄膜與基底之間的結(jié)合力。研究了退火對(duì)DLC薄膜性能的影響。采用中頻磁控濺射時(shí)引入了強(qiáng)磁陰極石墨靶,與普通陰極相比引入的磁性更強(qiáng),可以約束更多的電子去轟擊石墨靶材從而提高離化率和增強(qiáng)碳離子的濺射能量,增大了薄膜的沉積速率。系統(tǒng)地研究了濺射電流,氬氣流量和負(fù)偏壓對(duì)于薄膜性能的影響。得出了濺射電流為0.85 A,氬氣流量為20 sccm,負(fù)偏壓為50 V時(shí)制備的DLC薄膜的硬度性能最好,測(cè)出了硬度值為17.8 GPa,此時(shí)的薄膜與基底之間的結(jié)合力為18.48 mN。ECR-CVD引入了尖端放電原理制備DLC薄膜,目的是為了增大等離子體密度及試驗(yàn)一些極端實(shí)驗(yàn)條件對(duì)DLC薄膜成膜性能的影響。與普通方式下的ECR-CVD制備的DLC薄膜相比,整體的DLC薄膜的硬度性能更好。用ECR-CVD方法制備的DLC薄膜硬度可到達(dá)30 GPa左右,硬度值最高的為30.84 GPa,并且薄膜與基底之間的結(jié)合力為103.93 mN。所以得出ECR-CVD法制備DLC薄膜的硬度性能和薄膜與基底之間的結(jié)合力性能遠(yuǎn)好于磁控濺射法制備的DLC薄膜的硬度性能與薄膜基底之間的結(jié)合力。在工業(yè)應(yīng)用中,ECR-CVD法制備的DLC薄膜的硬度性能已經(jīng)可以達(dá)到作為硬質(zhì)涂層的硬度要求。退火處理使得DLC薄膜的表面產(chǎn)生一些裂紋,可能與退火溫度的選擇有關(guān)。退火溫度達(dá)到一定溫度的時(shí)候會(huì)有晶粒析出并且會(huì)產(chǎn)生脫落現(xiàn)象。DLC薄膜的SP3含量是隨著退火溫度的升高而減少的,因而導(dǎo)致DLC薄膜的硬度值與彈性模量都也隨著退火溫度的升高而減小。薄膜與基底之間的結(jié)合力在退火溫度為200°C時(shí)會(huì)有所增強(qiáng),當(dāng)退火溫度更高時(shí),薄膜與基底之間的結(jié)合力則會(huì)減弱。
[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 擄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.
【學(xué)位授予單位】:深圳大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類號(hào)】:TB383.2
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