One of the most important intermetallic compounds are titanium aluminides that given the importance and unique features such as low density, high strength, high melting point, and excellent corrosion and oxidation resistance and creep resistance at elevated temperatures Extensive research on the properties and overcome their weaknesses, to be used in various industries such as the aerospace industry has been studied. One of the most important weaknesses for this material is low toughness and ductility at room temperature that various solutions have been proposed such as The nanometer-scale materials produced by different manufacturing processes such as mechanical alloying, Microstructure control by selection of amount of aluminum and formation of two-phase microstructure (? 2 + ?) and Adding alloying elements in different amounts depending on the nature and properties. In this study, Ti-48at.% Al by mechanical alloying process at different times milling (30 and 70 hours) was produced. The results of X-ray diffraction (XRD) at this stage, shows the pure elements. In order to complete the formation of intermetallic compounds, heat treatment under vacuum and at 1000 ° C for 3 hours was performed. The test results (XRD) showed formation of intermetallic compounds such as TiAl, Ti 2 Al and Ti 3 Al and There is no any pure element. In another test, niobium (Nb) to increase strength and improve oxidation resistance at 3at.%., was added to the mix. X-ray diffraction test results after mechanical alloying at different times (30 and 70 hours) and after heat treatment, showes formation of Al 3 Nb on the side of titanium aluminide intermetallic compounds such as TiAl, Ti 2 Al and Ti 3 Al. According to grain size calculations by Williamson-Hall after mechanical alloying, and growth rate during the heat treatment, sample that 30 hours was mechanical alloyed with a grain size of about 47 nm in the alloy Ti-48at.% Al and about 41 nm in the Ti-48at.% Al-3at.% Nb was used to provide a bulk sample at 1000 ° C for 30 minutes. Scanning electron microscope (SEM) images of the surface, shows about 3% porosity. The test results (XRD) of surface, showed the formation of intermetallic compounds similar to heat treated samples. The oxidation test results at 1000 ° C for 70 hours, show better oxidation resistance in samples containing niobium so that the parabolic rate constant (K P ) calculated for Ti-48at.%Al 1.6329 and for Ti-48at.%Al-3at.%Nb 0.4223 respectively.