The synthesis and characterization of heterostructure por-Ga2O3/GaAs represent a crucial advancement in nanomaterials, particularly in optoelectronic applications. Employing a two-stage electrochemical etching methodology, this research has elucidated the precise conditions required to fabricate such a heterostructure. The initial stage involves etching monocrystalline gallium arsenide (GaAs) using an aqueous nitric acid solution as the electrolyte. This process is governed by the redox reactions at the crystal-electrolyte interface, where GaAs are partially oxidized and selectively etched. The second stage introduces ethanol into the electrolytic solution. This chemical addition serves a dual purpose: Firstly, it modulates the electrochemical environment, allowing for controlling pore morphology in GaAs. Secondly, it facilitates the etching of the resultant oxide layer, which predominantly consists of gallium oxide (Ga2O3). The formation of this oxide layer can be attributed to the oxidation of GaAs, driven by the electrochemical potentials and resulting in the deposition of reaction by-products on the substrate surface. The fabricated nanocomposite was comprehensively characterized using Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Analysis (EDX), and Raman Spectroscopy. SEM imaging revealed a range of agglomerated nanostructures dispersed across the surface, with dimensions ranging from 8–25 μm, 1–1.5 μm, and 70–100 nm. These observations suggest a hierarchical pore structure indicative of a complex etching mechanism modulated by the electrolyte composition. Raman spectroscopic analysis corroborated the presence of various phases in the heterostructure. Signals corresponding to bulk GaAs, serving as the substrate, were distinguishable. In addition, peaks indicative of porous GaAs and porous Ga2O3 were observed. A cubic phase in the Ga2O3 layer was particularly noteworthy, suggesting a higher degree of crystallinity. Notably, the absence of Raman-active modes associated with internal stresses implies that the fabricated heterostructure is of high quality.
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