Addressing the challenges in the synthesis and characterization of green photocatalysts is essential, and it is important to emphasize the need to combine various analytical techniques to obtain comprehensive and complete data. In this context, this chapter provides a comprehensive overview of methodologies and approaches for the synthesis and characterization of nanostructured photocatalysts, with a focus on efficiency and sustainability. Initially, a variety of approaches are presented for the synthesis and preparation of photocatalytic nanomaterials. Synthesis techniques, such as the sol-gel method, solvothermal, hydrothermal, polymer precursor method, chemical deposition techniques, and electrochemical methods, are explored, emphasizing the importance of selecting environmentally friendly solvents, reagents, and processes. Subsequently, it delves into the characterization approaches for the photocatalysts. Conventional and advanced techniques are analyzed, such as scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Rutherford backscattering spectrometry (RBS), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) surface area analysis, and ultraviolet-visible (UV-vis) spectroscopy. These techniques provide detailed insights into the photocatalysts’ physicochemical and morphological characteristics. This knowledge is crucial in advancing photocatalysis and charting a course for renewed efforts in environmental preservation and efficient energy usage.