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采用纳秒准分子激光在单晶硅试样表面制备了调制周期为50nm、调制比为2的TiN/AlN多层复合膜,并研究了N2分压对多层膜微结构和硬度的影响。结果表明,在低N2分压下薄膜表面颗粒相对较小,颗粒之间的空隙也不明显;随着N2分压的升高,薄膜表面颗粒明显粗化,且直径变大高度增高,颗粒之间孔隙变大。X射线衍射(XRD)研究表明,N2分压的增大可以在一定程度上促进AlN(002)相的形成,但抑制了TiN(111)的形成。X射线光电子能谱(XPS)研究显示,薄膜中N、Al、Ti元素有多种键合形式存在,并在界面形成TixAl1-xN复合。纳米硬度测量发现,N2分压的增大有利于薄膜硬度的提高,且薄膜硬度明显依赖于晶粒的尺寸分布和相结构。这一结果说明,纳秒准分子激光沉积制备TiN/AlN的过程中,通过控制N2分压调控激光等离子羽中粒子的运输能量不仅得到了预期的多层复合相结构,同时也调控了晶粒的尺寸分布。
The nano-scale excimer laser was used to prepare the TiN / AlN multilayer composite film with the modulation period of 50nm and the modulation ratio of 2 on the surface of monocrystalline silicon. The effect of N2 partial pressure on the microstructure and hardness of the multilayer film was also studied. The results show that the particles on the surface of the film are relatively small and the voids between the particles are not obvious under the low N2 partial pressure. With the increase of N2 partial pressure, the surface of the film is obviously roughened and the diameter increases and the height increases. Between the pores becomes larger. X-ray diffraction (XRD) studies show that the increase of N2 partial pressure can promote the formation of AlN (002) phase to a certain extent, but inhibit the formation of TiN (111). X-ray photoelectron spectroscopy (XPS) studies have shown that there are many kinds of bonding forms of N, Al and Ti elements in the film and form TixAl1-xN composite at the interface. The nano-hardness measurement shows that the increase of partial pressure of N2 is in favor of the increase of the hardness of the film, and the hardness of the film obviously depends on the size distribution and the phase structure of the crystal grain. This result shows that controlling the partial pressure of N2 to control the transport energy of the particles in the laser plume during the preparation of TiN / AlN by nanosecond excimer laser not only obtains the expected multilayered composite phase structure, but also regulates the crystal grain The size distribution.