This study focuses on the wet chemical synthesis of AlxGa1−xAs nanostructures, highlighting how different deposition conditions affect the film morphology and material properties. Electrochemical etching was used to texture GaAs substrates, enhancing mechanical adhesion and chemical bonding. Various deposition regimes, including voltage switching, gradual voltage increase, and pulsed voltage, were applied to explore their impact on the film growth mechanisms. SEM analysis revealed distinct morphologies, EDX confirmed variations in aluminum content, Raman spectroscopy detected structural disorders, and XRD analysis demonstrated peak position shifts. The findings emphasize the versatility and cost-effectiveness of wet electrochemical methods for fabricating high-quality AlxGa1−xAs films with tailored properties, showing potential for optoelectronic devices, high-efficiency solar cells, and other advanced semiconductor applications.