Layered double hydroxides with the hydrotalcite (Mg-(1-x)Al-x(OH)(2)(CO3)x/2.nH(2)O) structure intercalated with polyvanadate species have been prepared following different routes. X-ray diffraction, thermal analysis, transmission electron microscopy and infrared spectroscopy results indicate the layered structure of the material. A narrow mesopore size distribution was obtained when using terephtalate as swelling agent.