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采用磁过滤阴极真空弧技术(FCVA),以金属Zr为阴极靶,通入不同流速的C_2H_2和N_2气体(两者比例保持为1∶1),在单晶Si(100)晶面上制备nc-ZrCN/a-CN_x纳米复合薄膜。采用扫描电镜(SEM)、X射线衍射(XRD)、透射电镜(TEM)、X射线电子能谱(XPS)和拉曼散射能谱(Raman)多种材料分析技术研究薄膜的成分和结构。实验结果表明:薄膜是由两种相结构组成,分别为ZrCN纳米晶相(nc-ZrCN)和非晶相(a-CN_x);结构是由平均晶粒尺寸为5~12nm的nc-ZrCN弥散于非晶相a-CN_x中。纳米晶相nc-ZrCN中键态为Zr-C和Zr-N,非晶相aCN_x中键态为C-C,C=C和C-N。利用表面形貌仪(SM)和纳米力学探针(Nanotest)测量了薄膜的内应力、硬度和约化模量等力学性能。分析发现:薄膜中sp3和sp2的含量比(sp3/sp2)越大,内应力越大,内应力最大可达11.5GPa。ZrCN纳米晶粒细化和高的sp3/sp2含量比会提高薄膜的硬度和约化模量。当气流在15~35ml·min~(-1)范围时,薄膜具有很高的硬度和约化模量。当气流为25ml·min~(-1)时,硬度可达35.1GPa,约化模量达297.2GPa。
Using magnetic filtered cathode vacuum arc (FCVA) technology, metal Zr as cathode target, with different flow rate of C_2H_2 and N_2 gas (the ratio between the two kept 1: 1), prepared in the single crystal Si -ZrCN / a-CN_x nanocomposite films. The composition and structure of the films were studied by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray diffraction and X-ray Raman spectroscopy. The experimental results show that the film is composed of two phase structures, namely, ZrCN nanocrystalline phase (a-CN_x) and ZrCN nanocrystalline phase (a-CN_x); the structure is composed of nc-ZrCN dispersed with an average grain size of 5 to 12 nm In the amorphous phase a-CN_x. In the nanocrystalline phase nc-ZrCN, the key states are Zr-C and Zr-N, while the amorphous states aCN_x have C-C, C = C and C-N bonds. The mechanical properties of the film, such as internal stress, hardness and modulus of reduction, were measured by means of surface profilometer (SM) and nanotech probe (Nanotest). The results showed that the larger the sp3 and sp2 content ratio (sp3 / sp2), the larger the internal stress and the maximum internal stress of 11.5 GPa. ZrCN nano-grain refinement and high sp3 / sp2 content ratio will increase the film hardness and reduced modulus. When the airflow is in the range of 15 ~ 35ml · min ~ (-1), the film has high hardness and reduced modulus. When the airflow is 25ml · min ~ (-1), the hardness reaches 35.1GPa, and the reduced modulus reaches 297.2GPa.