The synthesis of metal oxide semiconductors has garnered considerable attention due to their wide-ranging applications in fields such as electronics, optoelectronics, catalysis, and photovoltaics. This study presents the synthesis of copper oxide nanoparticles (NPs) in distilled water through a two-probe electrochemical process at varying applied voltages. The synthesized copper oxide NPs exhibited a color spectrum from light to dark brown, suggesting the formation of copper oxide in the distilled water. Preliminary observations utilizing the Tyndall effect with a red laser light confirmed the colloidal nature of the solution. Photoluminescence emissions highlighted the semiconducting properties of the synthesized copper oxide NPs. The copper oxide NPs exhibited small size into quantum dots (QDs) at lower applied voltages, whereas higher voltages produced larger sizes. The appearance of ring-like patterns suggested a polycrystalline structure, which was further corroborated by selected area electron diffraction analysis, confirming the crystalline structure of Cu2O at low voltages and CuO at higher voltages. This study, therefore, demonstrates a straightforward method for synthesizing copper oxide using a two-probe electrochemical process, with the potential to produce QD and NP structures by modulating the applied voltage
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