Mladenović Ivana O, Lamovec Jelena S, Vasiljević-Radović Dana G, Vasilić Rastko, Radojević Vesna J, Nikolić Nebojša D
Institute of Chemistry, Technology and Metallurgy, University of Belgrade, Njegoševa 12, 11000 Belgrade, Serbia.
University of Criminal Investigation and Police Studies, Cara Dušana 196, Zemun, 11000 Belgrade, Serbia.
Materials (Basel). 2025 May 25;18(11):2480. doi: 10.3390/ma18112480.
The adhesion of copper thin films galvanostatically electrodeposited on Cu cathodes from electrolytes without or with the addition of various additives, such as chloride ions, polyethylene glycol 6000 (PEG 6000), and 3-mercapto-1-propanesulfonic acid, has been investigated. Morphological and structural analyses of synthesized films were performed using the SEM, AFM, and XRD methods, while the adhesion of the films was examined by applying the theoretical Chen-Gao (C-G) composite hardness model using results from Vickers microindentation, a bidirectional bending test, and a scratch-tape adhesion test. The morphologies of the films were either very smooth, with mirror-like brightness, obtained from the electrolyte containing all three additives, or microcrystalline, with different grain sizes, obtained from other electrolytes. The best adhesion was observed in the fine-grained film with numerous boundaries among grains, obtained with the addition of chloride ions and PEG 6000, while the mirror-bright film obtained with a combination of all three additives showed the worst adhesion. The boundaries among grains represented barriers that decreased the depth of penetration during microindentation and, consequently, increased the hardness and enhanced the adhesion of the film. The size of the grains-and hence, the number of grain boundaries-was regulated by the composition of the electrolytes achieved by the addition of additives. Good agreement was observed among the various methods used for the estimation of the adhesion properties of Cu films.
研究了在无添加剂或添加了各种添加剂（如氯离子、聚乙二醇6000（PEG 6000）和3-巯基-1-丙烷磺酸）的电解质中，在铜阴极上恒电流电沉积的铜薄膜的附着力。使用扫描电子显微镜（SEM）、原子力显微镜（AFM）和X射线衍射（XRD）方法对合成薄膜进行了形态和结构分析，同时通过应用理论上的陈-高（C-G）复合硬度模型，利用维氏显微压痕、双向弯曲试验和划痕胶带附着力试验的结果来检测薄膜的附着力。薄膜的形态要么非常光滑，具有镜面般的亮度，这是从含有所有三种添加剂的电解质中获得的；要么是微晶的，具有不同的晶粒尺寸，这是从其他电解质中获得的。在添加了氯离子和PEG 6000的情况下获得的具有许多晶粒间边界的细晶粒薄膜中观察到最佳附着力，而由所有三种添加剂组合获得的镜面光亮薄膜显示出最差的附着力。晶粒间的边界形成了屏障，减少了显微压痕过程中的穿透深度，因此提高了硬度并增强了薄膜的附着力。晶粒的尺寸以及因此晶粒边界的数量，由通过添加添加剂实现的电解质组成来调节。在用于评估铜薄膜附着力性能的各种方法之间观察到了良好的一致性。
