The synthesis of heteropolyacids-mesoporous silica composites was carried out in acidic media by impregnation and/or by direct incorporation of active phase. The effect of incorporation of heteropolyacids (HPAs) species into organized mesoporous silica was studied by using non-ionic and cationic surfactants. A comparison between direct incorporation of HPAs into mesoporous silica and impregnation of HPAs on mesoporous silica was done. The structure and texture of H(3)PMo(12)O(40) and H(4)PVMo(11)O(40) included on mesoporous silica were studied by XRD, SEM-EDS, FT-IR and Raman spectroscopies and BET and pore size distribution. Thermal stability was determined by thermo gravimetric analysis (TGA) and differential thermal analysis (DTA). FT-IR and Raman studies showed that HPAs anions preserved their Keggin structure after incorporation or impregnation on mesoporous silica support. (C) 2010 Elsevier Ltd. All rights reserved.