Powder profile studies in electrodeposited cuprous oxide films

Abstract

Thin films of copper oxide have been electrodeposited cathodically on copper substrates at room temperature. The deposited films have been characterized by X-ray diffraction and scanning electron microscopy. XRD showed the formation of crystalline cuprous oxide (Cu 2O). The XRD peaks are found to be shifted towards lower angle with narrowing of the profiles and the lattice parameter increases with annealing temperature. Scanning electron micrographs showed the formation of localized grain growth region which may be due to the non-uniform deposition of the films. The X-ray diffraction line broadening analysis of the as deposited as well as annealed films have been studied in order to evaluate the microstructural parameters which characterize the microstructural changes. The microstructural parameters like coherent domain size, RMS microstrain and dislocation density have been calculated using Warren-Averbach (Fourier) for multiple order, integral breadth (single and multiple line) and Williamson–Hall plot. The results of analysis obtained by different methods have been compared. The coherent domain size and RMS strain are not found to change appreciably with the increase of film thickness (4–13 μm). The optimum pH value of the electrolytic solution to deposit the films is found to lie in the range 9.2–9.3 where the strain variation is small compared to other pH values. The values of crystallite size and strains obtained by Warren–Averbach method and integral breadth method are comparable. However, Williamson–Hall plot overestimates the values of these two parameters. It is found that the crystallite size increases and RMS strain decreases with the increase of annealing temperature. The dislocation density is also found to decrease with annealing temperature.