Copper electrodeposition on (111)-oriented Si substrate was performed by the pulsating current (PC) regime at various average current densities in the range of 15-70 mA·cm −2 , obtained by varying either the frequency (30, 50, 80 and 100 Hz for the current density amplitude of 100 mA·cm −2 ) or the current density amplitude (120 and 140 mA·cm −2 at 100 Hz). The produced Cu coatings were examined by SEM, AFM and XRD techniques. The morphology of the coatings changed from those with large grains to fine-grained and globular, while the crystal structure changed from the strong (220) to the strong (111) preferred orientation by increasing the average current density. The mechanical characteristics of coatings were examined using Vickers micro-indentation tests, applying the Chicot-Lesage (C-L) composite hardness model for the analysis of microhardness. The maximum microhardness was obtained for the Cu coating produced at an average current density of 50 mA·cm −2 , with a current density amplitude of 100 mA·cm −2 and a frequency of 100 Hz. This copper coating was fine-grained and showed the smallest roughness in relation to the other coatings, and it was obtained in the mixed activation-diffusion control between the end of the effect of the activation control and the beginning of the dominant effect of diffusion control.

The mechanical characteristics of electrochemically deposited copper coatings have been examined by application of two hardness composite models: the Chicot-Lesage (C-L) and the Cheng-Gao (C-G) models. The 10, 20, 40 and 60 µm thick fine-grained Cu coatings were electrodeposited on the brass by the regime of pulsating current (PC) at an average current density of 50 mA cm−2, and were characterized by scanning electron (SEM), atomic force (AFM) and optical (OM) microscopes. By application of the C-L model we determined a limiting relative indentation depth (RID) value that separates the area of the coating hardness from that with a strong effect of the substrate on the measured composite hardness. The coating hardness values in the 0.9418–1.1399 GPa range, obtained by the C-G model, confirmed the assumption that the Cu coatings on the brass belongs to the “soft film on hard substrate” composite hardness system. The obtained stress exponents in the 4.35–7.69 range at an applied load of 0.49 N indicated that the dominant creep mechanism is the dislocation creep and the dislocation climb. The obtained mechanical characteristics were compared with those recently obtained on the Si(111) substrate, and the effects of substrate characteristics such as hardness and roughness on the mechanical characteristics of the electrodeposited Cu coatings were discussed and explained.

The influence of various electrolysis parameters, such as the type of cathode, composition of the electrolyte and electrolysis time, on the morphology, structure and hardness of copper coatings has been investigated. Morphology and structure of the coatings were analyzed by scanning electron microscope (SEM), atomic force microscope (AFM) and X-ray diffraction (XRD), while coating hardness was examined by Vickers microindentation test applying the Chicot–Lesage (C–L) composite hardness model. Depending on the conditions of electrolysis, two types of Cu coatings were obtained: fine-grained mat coatings with a strong (220) preferred orientation from the sulfate electrolyte and smooth mirror bright coatings with a strong (200) preferred orientation from the electrolyte with added leveling/brightening additives. The mat coatings showed larger both measured composite and calculated coating hardness than the mirror bright coatings, that can be explained by the phenomena on boundary among grains. Independent of electrolysis conditions, the critical relative indentation depth (RID) of 0.14 was established for all types of the Cu coatings, separating the zone in which the composite hardness can be equaled with the coating hardness and the zone requiring an application of the C–L model for a determination of the absolute hardness of the Cu coatings.

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Influence of annealing temperature on structural, optical and photocatalytic properties of TiO 2 -CeO 2 nanopowders, Ceramics International,