One step quickest mechanosynthesis of nanocrystalline Ti0.9Si0.1C and its microstructure characterization

Nanocrystalline Ti0.9Si0.1C has been prepared by ball-milling the elemental stoichiometric mixture of Ti, Si and graphite powders at room temperature under argon atmosphere. Microstructure characterization and quantitative estimation of different phases present in the unmilled and ball milled samples are done by analyzing the XRD patterns employing the Rietveld’s powder structure refinement method. The results reveal that formation of Ti0.9Si0.1C is initiated just after 44 min of milling and full formation of stoichiometric Ti0.9Si0.1C without any contamination is achieved within 3 h. To study the effect of ball milling on different microstructure parameters milling is continued up to 12 h which results in a reduction of particle size to ∼9 nm. Direct microstructure characterization of 12 h milled sample by HRTEM corroborates the structural and microstructural evolution by indirect method using XRD data.

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► Ti0.9Si0.1C (fcc) (>0.96 mol fraction) phase is noticed to form after 44 min of milling.
► Stoichiometric single phase Ti0.9Si0.1C without any contamination is formed within 3 h.
► HRTEM image confirms that nanoparticles are free from stacking faults.
► Both X-ray and HRTEM microstructure characterization reveal similar results.