Ti3SiC2 compound was synthesized by mechanical alloying (MA) using the starting materials consisting of 3Ti/Si/2C/0.2Al powder mixtures, and the effects of ball milling parameters (ball milling time, charge ratio, ball size, process control addition and attrition medium) on the MA synthesis of Ti3SiC2 were studied. The results show that, the powders and bulks product containing TiC and Ti3SiC2 were synthesized by chemical reaction between Ti, Si and C mixed powders after milling at ball size of 10 mm and ball-to-powder ratio of 10:1 for 7 h. Appropriate increase of ball size and charge ratio may obviously shorten the incubation period for reaction. However, using over large ball or high rate of ball-to-powder ratio will reduce the milling efficiency to extend incubation period. Adding alcohol as the process control addition (PCA) may not only prolong the incubation period, but also inhibit the synthesis of Ti3SiC2