Microstructure and phase transformation of Ti3AC2 (A = Al,Si) in hydrofluoric acid solution

In this paper, Ti₃AC₂ (A = Al, Si) were prepared by pressureless argon shielding synthesis technique. The microstructure and phase transformation of as‐prepared Ti₃AC₂ (A = Al, Si) in hydrothermal hydrofluoric acid (HF) solution were investigated systematically. Results showed that the obtained Ti₃AlC₂ and Ti₃SiC₂ were closely aligned layered structure. In hydrothermal HF solution, Al or Si element was preferentially etched from the layered structure, inducing obvious transformation of microstructure and phase composition. For Ti₃AlC₂, Al atoms diffused out of the structure and reacted with HF to form AlF₃•H₂O, which induced the rearrangement of the Ti and C atoms, and finally resulted in the formation of TiC_x cubic phase. With the hydrothermal temperature and reaction time increasing, the TiC_x phase gradually disappeared and the grain size of AlF₃•H₂O gradually increased. When Ti₃SiC₂ was immersed in hydrothermal HF solution, the main products were TiC and SiC. Interestingly, with the hydrothermal treatment temperature and reaction time increasing, TiC gradually disappeared, while SiC nearly kept unchanged. This can be explained that SiC was covalently bonded carbide, while TiC was metallically bonded, having relatively weak bond energy and consequently being unstable in hydrothermal HF solution.