Titanium and zirconium oxides with interconnected macropores presenting well-defined pore sizes and controlled three-dimensional ordering were prepared using a latex templating method. Polystyrene spheres were used as pore templates, whereas metal alkoxides were used as oxide precursors. The final thermal treatment at different temperatures showed macroporous microstructure stabilities up to 600 degrees C. At higher temperatures, a collapse of the macroporous microstructure and sintering were observed, as well as phase transformations in the oxides structures during the calcination process, as shown by Raman spectroscopy and X-ray diffraction techniques.