An efficient approach has been developed to synthesize a new versatile organo-silica material by non-conventional method (microwave irradiation and ultrasonic vibration) from amorphous pyrogenic silica and has been compared with thermic procedure. The samples were fully characterized by FTIR, solid-state Si-29 and C-13 CP/MAS NMR, thermogravimetric analysis (TGA), elemental analysis, scanning electron microscopy (SEM) and by N-2-sorption isotherms measurements. The functionalization of silicon dioxide by 4-(chloromethylphenyl) trichlorosilane has been easily achieved by ultrasound irradiation in a very short time with high loading of organic fragments. Significant different sizes of pores were observed according to conventional or non-conventional synthesis procedure. In addition, new structural properties have been created with the emergence of a mesoporosity. (C) 2010 Elsevier Inc. All rights reserved.