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采用磁控溅射技术在钛合金和单晶Si上沉积原子分数x(Al)分别为5%、23%、47%、63%的ZrAlN薄膜,并考察了薄膜硬度和断裂韧性。采用场发射扫描电镜观察截面形貌,X射线衍射(X-Ray Diffraction,XRD)分析物相结构。采用纳米压入仪进行10 mN加载、卸载试验,分析了薄膜的弹塑性变形特性;采用压入法定量比较了薄膜的断裂韧性。试验发现:原子分数x(Al)分别为5%、23%、47%、63%的ZrAlN薄膜对应硬度分别为24.5、40.1、17.1、19.1 GPa;对应断裂韧性分别为1.47、3.17、1.13、1.58 MPa·m1/2;x(Al)=23%的薄膜保持了ZrN的金属键特性,韧性最好;而x(Al)=47%的薄膜表现强烈离子键特性,韧性最差。XRD表明:x(Al)分别为5%和23%时,Al原子固溶到ZrN晶粒中,保持ZrN立方结构;而x(Al)分别为47%和63%时,形成纤锌矿AlN第二相。
The ZrAlN films with 5%, 23%, 47% and 63% atomic fraction x (Al) were deposited on titanium alloy and monocrystalline Si by magnetron sputtering. The hardness and fracture toughness of the films were also investigated. The morphology of the cross section was observed by field emission scanning electron microscopy and the phase structure was analyzed by X-ray diffraction (XRD). The loading and unloading tests of 10 mN were carried out by nanoindenter, the elasto-plastic deformation characteristics of the film were analyzed, and the fracture toughness of the film was compared quantitatively by using press-in method. The experimental results show that the corresponding hardness of ZrAlN films with the atomic fraction x (Al) of 5%, 23%, 47% and 63% are 24.5, 40.1, 17.1 and 19.1 GPa respectively; the corresponding fracture toughnesses are 1.47, 3.17, 1.13 and 1.58 The film with x (Al) = 23% retained the metallic bond of ZrN with the best toughness. However, the film with x (Al) = 47% showed the strong ionic bond with the worst toughness. The results of XRD show that the Al atoms are dissolved into the ZrN grains at 5% and 23%, respectively, and maintain the ZrN cubic structure. When x (Al) is 47% and 63%, respectively, the wurtzite AlN Second phase