<p>This study focuses on the fabrication and characterization of ZrO₂‒TiO₂ mixed oxides modified with gallium and surfactants and their potential application as supports for NiW hydrodesulfurization (HDS) catalysts. The mixed oxides were synthesized via the soft template sol‒gel method with the incorporation of triblock copolymers as surfactants (P123 and L64). We focus on the incorporation of gallium into the supports to modify their surface properties and acidity. The NiW catalysts were evaluated in the HDS of dibenzothiophene (DBT) under high pressure conditions. The results demonstrated that the incorporation of surfactants induced an increase in surface area and an improvement in pore structure within the oxides, which in turn led to enhanced dispersion of the active phases. Additionally, gallium facilitated the sulfidation of the W species and the formation of the NiWS active phase. The catalytic test demonstrated that the catalyst prepared with surfactants, particularly the NiW/ZT-P-Ga catalyst, exhibited the highest initial reaction rates and selectivity toward the hydrogenation pathway. The study demonstrated that the combination of surfactants and gallium ions in the preparation of ZrO₂–TiO₂ supports can significantly enhance the performance of NiW catalysts for deep desulfurization. These findings contribute to the development of more efficient catalysts for industrial HDS processes, addressing the challenges posed by refractory sulfur compounds in fuels.</p>