The synthesis and characterization of TiO2 macrocellular scaffolds was describe using a rational air-liquid foaming sol-gel process. It was observed that apart from the macroscopic-shape control, Plateau-border thicknesses and lengths can be tuned, almost on demand. A process was developed that allows a high degree of control over the macroscopic cell sizes and morphologies of silica foam. In order to search for a higher mesoporosity, synthesis with Tergitol was performed at different weight fractions.