This paper describes how the preparation and heat treatment of TiC/Si powders influences the phase reactions during firing. The powders are prepared by milling and some effects of powder preparation are discussed. A solid state displacement reaction according to: 3TiC + 2Si → Ti3SiC2 + SiC is a priori expected to take place during heat treatment. The firing procedure is investigated with respect to the effect of heat treatment time and temperature on the phases produced, especially Ti3SiC2. Samples were heat treated in a graphite lined furnace. Heat treated samples are analysed by x-ray diffraction, scanning electron microscope and energy dispersive spectroscopy. Ti3SiC2, TiC and SiC are dominant in the final products. The highest amount of Ti3SiC2 is achieved for short holding times (2-4 hours) at high temperatures (1350-1400°C). Ti3SiC2 appears to decompose at elevated temperatures or extended times, through a Ti3SiC2 → TiC + Si(g) type reaction. The activation energy of Ti3SiC2 phase formation is determined to be 289 kJ/mol, using the Mehl-Avrami-Johnson model.