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用磁控共溅射法制备含铌1.16%～27.04%(原子分数)的Cu-Nb合金薄膜,运用EDX,XRD,SEM,TEM,显微硬度仪和电阻仪对沉积态和热退火态薄膜的成分、结构和性能进行了研究。结果表明,Nb添加显著影响Cu-Nb合金薄膜微结构,使Cu-Nb薄膜晶粒细化,含铌1.82%～15.75%的Cu-Nb膜呈纳米晶结构,存在Nb在Cu中的fcc Cu(Nb)非平衡亚稳过饱和固溶体,固溶度随薄膜Nb浓度增加而上升,最大值为8.33%Nb。随Nb含量增加,薄膜中微晶体尺寸减小,Cu-27.04%Nb膜微结构演变至非晶态。与纯Cu膜对比表明,Nb添加显著提高沉积态Cu-Nb薄膜显微硬度和电阻率,总体上二者随膜Nb含量上升而增高。Nb含量高于4.05%时显微硬度增幅趋缓,非晶Cu-Nb膜硬度低于晶态膜,电阻率则随铌含量上升而持续增加。经200,400及650℃退火1h后,Cu-Nb膜显微硬度降低、电阻率下降,降幅与退火温度呈正相关。XRD和SEM显示,650℃退火后晶态Cu-Nb膜基体相发生晶粒长大,并出现亚微米级富Cu第二相,非晶Cu-27.04%Nb膜则观察到晶化转变和随后的晶粒生长。Nb添加引起晶粒细化效应以及退火中基体相晶粒度增大是Cu-Nb薄膜微观结构和性能形成及演变的主要原因。
The Cu-Nb alloy films containing niobium from 1.16% to 27.04% (atomic fraction) were prepared by magnetron sputtering. The deposited and annealed films were characterized by EDX, XRD, SEM, TEM, The composition, structure and properties were studied. The results show that the addition of Nb significantly affects the microstructure of the Cu-Nb alloy film and the grain refinement of the Cu-Nb thin film. The Cu-Nb film with Nb ranging from 1.82% to 15.75% exhibits nanocrystalline structure with fcc Cu (Nb) non-equilibrium metastable supersaturated solid solution, the solid solubility increases with the increase of Nb concentration, the maximum value is 8.33% Nb. With the increase of Nb content, the crystallite size decreases and the microstructure of Cu-27.04% Nb film evolves to amorphous state. Compared with the pure Cu film, Nb addition significantly increased the microhardness and resistivity of the as-deposited Cu-Nb film, and both increased with increasing Nb content. When the Nb content is higher than 4.05%, the microhardness increases slowly, the hardness of the amorphous Cu-Nb film is lower than that of the crystalline film, and the resistivity increases continuously with the increase of niobium content. After annealed at 200, 400 and 650 ℃ for 1h, the microhardness of Cu-Nb films decreased and the resistivity decreased. The decrease was positively correlated with the annealing temperature. XRD and SEM showed that the grain growth of the crystalline Cu-Nb film occurred after 650 ℃ annealing, and the submicron Cu-rich second phase appeared. The amorphous Cu-27.04% Nb film then observed the crystallization transformation and then Of the grain growth. The main reason for the formation and evolution of the microstructure and properties of the Cu-Nb thin films is the grain refinement effect caused by Nb addition and the grain size increase of the matrix during annealing.