The regular iron nanoparticles embedded in the mesoporous silica SBA-15 walls was synthesized using a classical impregnation modified by ultrasonication and microwave procedure. Iron nanoparticles in mesoporous silica (IMS) with ordered hexagonal structure were prepared by using mesoporous silica SBA-15 as a template and iron nitrate as an iron precursor. The character of material during synthesis investigated by several such as energy dispersive X-ray (EDAX), X-raydiffraction (XRD), Fourier Transformation Infra Red Spectroscopy (FTIR), Differential Thermal Analysis-Differential Scanning Calorimetry (DTA-DSC), nitrogen adsorption-desorption and transmission electron microscopy (TEM).The results show that IMS materials after the calcination at 700 ºC have a good thermal stability under nitrogen at 750 ºC. Nevertheless, ultrasonication and microwave treatment during impregnation process enhanced the affinity between silica and iron functional group through silanol ways. The iron addition after ultrasonication leads to large iron content in mesoporous silica while the silanol group is slightly increased during the calcination. Different from ultrasonication, microwave treatment renders a continuous increase of iron content as well as the total element with increasing the silica calcination. After calcination treatment at 700 ºC, the regular mesostructures destruction occurred due to the fast thermal reactions between silica and oxygen

Key word: iron nanoparticle, mesoporous silica, ultrasonication, microwave