Ultrafast one step mechanosynthesis of nanocrystalline cubic Ti0.9Si0.1B and its microstructure characterization

Nanocrystalline cubic Ti0.9Si0.1B phase has been prepared by mechanical alloying the stoichiometric mixture of Ti, Si and boron powders at room temperature in a planetary ball mill under argon atmosphere. Microstructure characterizations of unmilled and all ball-milled powders in terms of lattice imperfection are made by analyzing respective X-ray diffraction data employing the Rietveldʹs powder structure refinement method. It reveals that after 1 h of milling, α-Ti (hcp) phase is partially transformed to metastable β-Ti (bcc) phase and the initiation of Ti0.9Si0.1B phase takes place. Contamination free stoichiometric nanocrystalline cubic Ti0.9Si0.1B phase is synthesized within 3 h of milling with ∼ 3 nm particle size. Microstructure characterization of 17 h milled sample by high resolution transmission electron microscopy (HRTEM) reveals that the average size of almost mono-dispersed spherical particles is ~ 5 nm which corroborates the finding of the Rietveld analysis.