Preparation of TiC/Ti3SiC2 Composite by Sintering Mechanical Alloyed Ti–Si–C Powder Mixtures

The present work aims to evaluate the crystalline phases and microstructure of a TiC–Ti3SiC2 ceramic composite, obtained by mechanical alloying of Ti, C and Si powders and subsequent sintering. A mechanical alloying technique in a planetary ball mill for 1, 10, 50, 100 and 200 h using Ti, Si and C powders with molar ratios of 3:1:2 as feedstock in argon (Ar) gas was employed to prepare nano-sized Ti–Si–C powders. TiC crystallite size and lattice strain were evaluated by X-ray diffraction analysis (XRD) and the morphological characteristics and particle size distribution were examined using scanning electron microscope (SEM). After milling, a reduction of the average particle size and crystallinity is observed. Furthermore, after 10 h of milling time, TiC starts to crystallize. The powder mixture obtained after 200 h of milling was compacted and sintered at 1200 °C under controlled atmosphere, for 15 min, 2 h or 4 h with a heating rate of 5 °C/min. Almost full densification of samples sintered for 2 h and 4 h has been achieved, with relative densities close to 98.8±0.2% and TiC and Ti3SiC2 as crystalline phases with an average crystallite size of TiC near 0.7 μm. Rietveld refinement indicates that the majority TiC-cubic phase (>85 vol%) presents a unit cell volume of 8.03 nm3 after sintering at 1200 °C. Despite the maintenance of the volume of the hexagonal unit cell of Ti3SiC2, (15.05 nm3), the increase of the isothermal sintering time resulted in an increase of the lattice parameter “a”, from 0.315 nm to 0.320 nm, and a reduction of the lattice parameter “c” from 1.750 nm to 1.705 nm. The control of the changes in the residual stresses within the TiC matrix and the Ti3SiC2 precipitates, which is associated with the deformation in the lattice parameters, must be controlled to achieve high fracture toughness in the composite.