In-situ high temperature annealing of nanostructured ZrTiO4 prepared by mechanical alloying

High-energy ball-milling of monoclinic (m) ZrO2–anatase (a)TiO2 mixture (3:2 molar ratio) at room temperature results in partial formation of nanocrystalline orthorhombic ZrTiO4 phase after 8 h of milling. ZrTiO4 phase is formed from the high pressure srilankite (s)-TiO2 based TiO2–ZrO2 solid-solution. In-situ high temperature annealing of ZrTiO4, m-ZrO2 and a-TiO2 powder mixture results in complete transformation of ZrTiO4 at 1073 K. Microstructure characterization of the ball-milled and in-situ annealed samples in terms of several lattice imperfections is made employing the Rietveld’s method of structure refinement using X-ray powder diffraction data. Phase transformation kinetics and in addition to microstructure parameters, relative phase abundances of different phases are revealed from the Rietveld analysis. The analysis reveals that the ZrTiO4 is formed from the isostructure s-TiO2 based TiO2–ZrO2 solid-solution with ∼11 nm particle size after annealing at 1073 K.