The interpenetrating 3-dimensional channel system of silica MCM-48 has been selected for the deposition of ZnO nanoparticles. The post-synthetic organometallic route was employed to load the mesoporous silica with ZnO-precursor molecule. Calcination of the composite transformed the organometallic sorbate to the corresponding metal oxide. X-ray powder diffraction, N2-Adsorption and TEM measurement have supported the efficient loading and growth of ZnO particles in the channels of mesoporous silica matrix. EXAFS analysis (ZnK-edges) also complemented the metal uptake. Presence of nano-dispersed and nanosized ZnO particles confined by the mesoporous pore system was established by TEM and EXAFS analysis.