A sustainable method of hydrogen production for use as a fuel for energy generation is one area of research aimed at reducing carbon emissions from fossil fuels. This H₂ can, in principle, be supplied by the photocatalytic splitting of water, using sunlight. Titanium dioxide is a well known photocatalyst sensitive to UV wavelengths, and can be activated for visible light absorption with the use of photosensitive materials and dyes. A mesoporous TiO₂ aerogel was prepared by means of a sol-gel process followed by solvent extraction with a supercritical (SC) solvent, such as ethyl acetate or ethanol. In this way it was possible to synthesize a material with a large surface area, and use this porous structure as a support for CdS nanoparticles, a catalyst sensitive to visible light, having a lower bandgap than that of TiO₂. Studies on the effect of different SC solvents and the performances of the material in the photogeneration of H₂ are reported.