FERRIC CHLORIDE CHLORINATION OF TITANIUM NITRIDE AT LOW TEMPERATURE

Abstract

In this study, the effects of soaking temperature and time on the low-temperature Ferric chloride (FeCl3) chlorination process of pure titanium nitride (TiN) have been investigated. Chlorination temperatures ranged from 200–400°C for 1–3 hours. Statistical analysis of the results was done by Design of Experiment (DOE) to identify the associated dominating variables and their interactions. From DOE analysis, a soaking time of 3 hours at 400°C was found to have maximum extraction extent of titanium (XTi) of ~ 72.6%. The lowest XTi was 55.3% that was obtained at 200°C for 1 hour. Perturbation plots showed both temperature and soaking time affected XTi. From the perturbation plots of XTi, both temperature and soaking time gave positive effects on chlorination with soaking time giving the highest impact. X-ray diffraction (XRD), scanning electron microscopy and energy dispersive X-ray analysis (SEM/EDX) were conducted to evaluate the morphology of TiN and chlorination residues. The results showed gradually amorphous phase formation from unchlorinated TiN powder. The utilization of FeCl₃ as a chlorination agent was feasible and showed good extraction of titanium at 400°C.