<p>This study investigates the influence of preparation methods on the physicochemical and catalytic properties of CuAlOx bimetallic oxides (Cu/Al = 1). Two preparation methods were investigated: sol–gel (CuAl-SG) and hydrothermal (CuAl-Hyd). Characterization by XRD, BET-BJH, and SEM revealed significant differences in structure, texture, and catalytic performance. XRD analysis showed that CuAl-Hyd forms separate CuO and Al₂O₃ phases, whereas CuAl-SG produces CuAlO₂ with a hexagonal delafossite structure. BET analysis indicated that the surface area of CuAl-Hyd is 80% larger than that of CuAl-SG. However, CuAl-SG exhibits a more homogeneous pore distribution, lower pore volume, and larger average pore diameter. SEM imaging revealed that CuAl-Hyd forms smaller, more uniformly distributed particles with lower crystallinity, whereas CuAl-SG results in agglomerated particles. Catalytically, both systems showed high activity in isopropanol decomposition. CuAl-SG displayed stronger redox properties, whereas CuAl-Hyd exhibited enhanced acid–base characteristics. In benzaldehyde reduction, CuAl-SG achieved higher conversion and selectivity for benzyl alcohol, attributed to the presence of Cu⁺ in the delafossite CuAlO₂ structure. Its uniform pore distribution and larger average pore diameter also facilitate desorption of benzylate intermediates, thereby improving selectivity. This study highlights the crucial role of synthesis methods in tuning the structural, textural, and catalytic properties of CuAlOx. These findings provide insights into the design of efficient catalysts for specific reactions and emphasize the importance of preparation techniques in optimizing performance.</p>