Titanium Aluminide-based composites with Al2O3 reinforcement can be produced via reaction of Al with TiO2. These composites are considered as low-cost materials for high temperature applications. Addition of KClO4 to the TiO2/Al system was investigated in this research. On the basis of the results obtained, addition of KClO4 to the mixture of TiO2/Al and subsequent heating, results in titanium aluminide/alumina nanometric particle formation with dimensions of about 30 nm. Densification of this composite powder leads to production of a titanium aluminide-alumina nanocomposite body. Dimensions of the alumina phase are in the range of 100-150nm.