In this study Ti₃SiC₂ MAX phase synthesized by mixing of Ti, Si and C powders and mechanical alloying - heat treatment. The composition of 3Ti:1.3Si: 2C were used in order to evaluate the milling time and also heat treatment temperature in synthesis of Ti₃SiC₂ MAX phase. At first the initial powders were weighed and mechanical alloying was carried out using ball to the powder ratio of 50:1 for 30, 40 and 50 hours under argon atmosphere. Then the mixed powders were pressed in steel mold with the diameter of 1.2 cm to shape discs under the pressure of 200 MPa. After a complementary heat treatment of the samples at 1100, 1200 and 1300 °C for 1 hour, an X-ray diffraction analysis was used to examine phase composition while a field emission transmission electron microscope equipped with an EDS spectrometer was utilized to observe the microstructure. Finally, it was found that the maximum amount of the synthesized Ti₃SiC₂ MAX phase is totally equal to 75wt.%  which is related to the sample with milling time of 40 hours and heat treated at the temperature of 1200°C. It was also observed that the weight percentage of the Ti₃SiC₂ MAX phase has decreased in the reaction products by increasing of the milling time from 40 to 50 hours.