An experimental study of the deposition of Ti3SiC2-based ceramics from TiCl4-SiCl4-CH4-H-2 gaseous precursors is carried out under conditions chosen on the basis of a previous thermodynamic approach, i.e. a temperature of 1100-degrees-C, a total pressure of 17 kPa, various initial compositions and substrates of silicon or carbon. Ti3SiC2 is deposited within a narrow composition range and never as a pure phase. A two-step deposition process is observed, in agreement with the thermodynamic calculations. For a silicon substrate, TiSi2 is formed as an intermediate phase from consumption of Si by TiCl4 and then is carburized by CH4 into Ti3SiC2. For a carbon substrate, the first step is the formation of TiC(x) either from consumption of carbon by TiCl4 or by reaction between TiCl4 and CH4 and then TiC(x) reacts with the gaseous mixture to give rise to Ti3SiC2. In most cases, Ti3SiC2 is obtained as small hexagonal plates oriented perpendicular to the substrate surface. These nano- or micro-crystals are usually co-deposited with TiC(x) and to a lesser extent SiC, and their size is increased by increasing the dilution of the gaseous mixture in hydrogen.