MXene phases are bi-dimensional carbide or nitride phases with original properties that have generated interest in domains such as energy storage [1,2], electronics [3,4] or even catalysis [5]. These phases are synthesized by ablation of MAX phases whose composition flexibility leads to the optimization of their properties and those of the associated MXene phases. In this study, synthesis of the M2AlC MAX phase by arc discharge and Spark Plasma Sintering (SPS) from M (transition metal: Ti, Zr or Hf), Al and MC powders have been carried out. To increase the proportion of the target-phase in the samples and limit the proportion of secondary phases, the synthesis parameters have been optimized. The optimization of the intensity of the arc and duration of the heating in the electric arc furnace were carried out to obtain the desired composition, i.e. to limit the proportion of secondary intermetallic and carbide phases. By using SPS, the sintering cycle was imagined in two parts: a first hold, at a relatively low temperature to limit the aluminum vaporization, to allow for the formation of intermetallic phases from the elemental M and Al powders, which can then react during the second hold at higher temperatures with the MC powder to form the carbide MAX phase. The temperature, holding time and load applied were optimized to limit the formation of unwanted phases. Pressure-less cycles, where no load was applied to the sample during the sintering, were also studied. In the Ti-Al-C system, the samples synthesized by arc discharge contained up to 60 wt.% of the 211 phase. Nevertheless, the 312 phase was always present as a secondary phase, alongside TiC. By using SPS, a sample containing only the 211 phase was obtained through the pressure-less cycle. It was composed of a first hold at 600 °C for 15 min and a second one at 1200°C for 10 min. In the case of load application (75 MPa), the best sample contained around 87 % of the Ti2AlC phase and was fabricated with the same temperature cycle as above. Experiments regarding the synthesis of the Zr- and Hf- containing MAX phases are still on-going. [1] Q. Tang, Z. Zhou, P. Shen, J. Am. Chem. Soc. 134 (2012) 16909–16. doi:10.1021/ja308463r [2] D. Er, J. Li, M. Naguib et al., ACS Appl. Mater. Interfaces. 6 (2013). doi:10.1021/am501144q [3] J. Halim, M. Lukatskaya, K. Cook et al., Chem. Mater. Publ. Am. Chem. Soc. 26 (2014) 2374–2381. doi:10.1021/cm500641a [4] V. Mauchamp, M. Bugnet, E.P. Bellido et al., Phys. Rev. B. 89 (2014) 235428. doi:10.1103/PhysRevB.89.235428 [5] X. Xie, S. Chen, W. Ding et al., Chem. Commun. Camb. Engl. 49 (2013). doi:10.1039/c3cc44428g