The fission-product 99 Mo, having a high specific activity, is commonly used in alumina-based 99 Mo /99m Tc generator. Due to the limitation on the use of fissionproduct 99 Mo, an alternative route for 99 Mo production, namely activation of natural molybdenum using thermal neutron, has been explored. Unfortunately, this neutronactivated 99 Mo has a low specific activity. Therefore, 99 Mo /99m Tc generator based on neutron-activated 99 Mo requires a column with higher capacity absorbent. Thus, in this study, the nanomaterial of alumina (nano--Al2O3) was synthesized which was expected to have a higher 99 Mo adsorption capacity, so that nano--Al2O3 could be potentially used as a matrix of column for 99 Mo/ 99m Tc generator based on neutron-activated 99 Mo. Nano--Al2O3 was synthesized by using sol-gel method and characterized using FTIR spectroscopy, X-ray diffraction (XRD), and transmission electron microscopy (TEM). In addition, the Scherrer method was used to determine the size of the crystals. To determine the 99 Mo adsorption capacity of the synthesized nanoalumina, the nano--alumina was soaked in nitric acid solution for one hour at room temperature followed by removing the filtrate. Then, the nano--alumina was soaked in 99 Mo solution (Na2 99 MoO4) at certain conditions. The FTIR spectra for nano--alumina showed adsorption peak at 450-500 cm -1 which indicated the presence of Al-O bond. The XRD patterns of nanoalumina crystals showed peaks at 2θ region of 25.8°, 35.9°, 38°, 52.8°, and 57.7°, indicating that the synthesized alumina had an α-phase with an average crystal size of ~5.5 nm. The average 99 Mo adsorption capacity of the synthesized alumina was 47.55 ± 12.3 mg Mo/g nano--Al2O3.