Nanostructured silica and silica-iron composite particles were prepared using water-in-oil (w/o) reverse microemulsion. Double microemulsion technique is used for the synthesis of both types of nanostructured particles. X-ray Diffractometry (XRD), scanning electron microscopy (SEM), nitrogen gas adsorption-desorption isotherm technique, and differential scanning calorimetry (DSC) were used to characterize the synthesized particles. The gas adsorptiondesorption measurements revealed a mesoporous structure for the silica (SiO2) particles with a surface area of 300.49 m2/g. Upon the addition of an iron microemulsion to the silica microemulsion, silica-iron nanocomposite (Fe2O3-SiO2) was achieved which gave a surface area of 69.87 m2/g. This indicated a positive impregnation of the silica mesopores that was further confirmed by energy dispersive spectrometry (EDS). The XRD of bare SiO2 gave a single broad peak whereas SiO2-Fe2O3 demonstrated additional peaks confirming α-iron insertion in mesoporous silica. DSC curve with its characteristic peaks also indicated the presence of iron nanoparticles within silica. The product silica-iron nanocomposite has potential catalytic and semiconducting applications.