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

J Nanosci Nanotechnol. 2020 Jul 1;20(7):4580-4586. doi: 10.1166/jnn.2020.17869.

Abstract

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.