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采用磁控溅射技术在钛合金和单晶硅上沉积ZrCuN薄膜,考查了正负脉冲偏压对薄膜微观结构和硬度、韧性的影响。采用场发射扫描电镜观察截面形貌,X射线光电子能谱(XPS)分析元素结合状态,X射线衍射(XRD)分析物相结构。采用纳米压入仪进行加载、卸载试验,分析了薄膜弹塑性变形特性;采用压入法定量比较了薄膜的断裂韧性。结果表明:正偏压不影响薄膜结构,其效果在于提高沉积速率约20%,改变等离子体内电荷状态,从而改变了薄膜的成分。向ZrN中添加少量Cu,抑制了柱状晶,薄膜结构由T区向II区转变;ZrN薄膜中加入Cu后硬度并未降低,而韧性得到很大改善。Cu在薄膜中以2种形式存在:一是替换固溶到ZrN晶粒中;二是以单质Cu存在于晶界。
The ZrCuN films were deposited on titanium alloy and monocrystalline silicon by magnetron sputtering. The effects of positive and negative pulse bias on the microstructure, hardness and toughness of the films were investigated. The morphology of the cross section was observed by field emission scanning electron microscopy, the elemental binding state was analyzed by X-ray photoelectron spectroscopy (XPS) and the phase structure was analyzed by X-ray diffraction (XRD). The nano-indenter was used to carry out the loading and unloading tests, and the elasto-plastic deformation characteristics of the film were analyzed. The fracture toughness of the film was compared quantitatively by using the press-in method. The results show that the positive bias does not affect the structure of the thin film. The effect is to increase the deposition rate by about 20% and change the charge state in the plasma to change the composition of the thin film. Addition of a small amount of Cu into ZrN suppresses the columnar crystal, and the film structure changes from T zone to II zone. The hardness of ZrN film does not decrease but the toughness is greatly improved. Cu exists in two forms in the film: one is to replace the solid solution into the ZrN grains; the other is to exist as a single Cu at the grain boundaries.