Self-propagating high-temperature synthesis of Ti3SiC2:: I, ultra-high-speed neutron diffraction study of the reaction mechanism

In situ neutron diffraction at 0.9 s time resolution was used to reveal the reaction mechanism during the self-propagating high-temperature synthesis (SHS) of Ti3SiC2 from furnace-ignited stoichiometric 3Ti + SiC + C mixtures. The diffraction patterns indicate that the SHS proceeded in five stages: (i) preheating of the reactants, (ii) the alpha --> beta phase transformation in Ti, (iii) preignition reactions, (iv) the formation of a single solid intermediate phase in <0.9 s, and (v) the rapid nucleation and growth of the product phase Ti3SiC2. No amorphous contribution to the diffraction patterns from a liquid phase was detected and, as such, it is unlikely that a liquid phase plays a major role in this SHS reaction. The intermediate phase is believed to be a solid solution of Si in TiC such that the overall stoichiometry is similar to3Ti:1Si:2C. Lattice parameters and known thermal expansion data were used to estimate the ignition temperature at 923 +/- 10degreesC (supported by the alpha --> beta phase transformation in Ti) and the combustion temperature at 2320 +/- 50degreesC.