This work aims to produce Ti3AlC2 powder via a new route that consists of two-step processes, and studies the sintering kinetics and effect of nickel addition on the pressureless sintering behavior of Ti 3AlC2 powder. Ti3AlC2 powder of about 5 μm was produced using TiCx and Al powder. Relative density of about 97.6% was achieved using 1 wt% nickel as a sintering aid. Ti 3AlC2 powder shows two different activation energies (AE) of sintering, 347 ± 4 and 183 ± 8 kJ/mol at lower and higher temperature ranges, respectively. These AE were found to be matching closely with the AE of Al diffusion in the Ti-Al binary system reported in the literature, indicating that the sintering of ternary Ti3AlC 2 ceramic was controlled by the diffusion of Al atoms. When nickel is added, Ni reacts with Ti3AlC2, tends to decompose it, and forms Ni-based compounds and liquid phase. Nickel was found to suppress the grain growth of Ti3AlC2 significantly. Sintered sample exhibited a Vickers hardness of 3.2 GPa at a load of 10 N. © 2010 The American Ceramic Society.