Preparation and microstructure characterization of m-ZrO2-20 mol% a-TiO2 ball milled mixture by Rietveld method

High energy ball milling of monoclinic (in) ZrO2-20 mol% anatase (a) TiO2 mixture at different durations, results in formation of m-ZrO2-a-TiO2 solid solution from which the nucleation of nanocrystalline cubic (c) ZrO2 polymorphic phase sets in. Post-annealing of 12 h ball milled sample at different elevated temperatures for 1 h results in almost complete formation of c-ZrO2 phase. Microstructure of the unmilled, all ball milled and post-annealed samples has been characterized by employing Rietveld's X-ray powder structure refinement methodology. Particle size, r.m.s. lattice strain, lattice parameters, molar fraction etc. of individual phases have been estimated from Rietveld analysis and are utilized to interpret the results. Cubic phase is presumed to have formed on the (001) of the m-ZrO2-a-TiO2 solid solution. In course of milling, most dense (111) of cubic lattice became parallel to most dense ((1) over bar 11) of monoclinic lattice due to lattice orientation effect. Annealing of 12 h ball milled sample at 773, 873, 973 and 1073 K each for I h duration results in reduction of lattice strain to a considerable amount and negligible increase in particle size of both the m- and c-ZrO2 phases. It suggests that almost fully stabilized nanocrystalline c-ZrO2 can also be formed by adding a tetravalent solute to m-ZrO2. (C) 2003 Elsevier B.V. All rights reserved.