Microstructure evolution of an equimolar powder mixture of ZrO2–TiO2 during high-energy ball-milling and post-annealing

Preparation of nanostructured ZrTiO4 by solid state reaction in equimolar mixture of TiO2 and ZrO2

“…The conditions in our experiment resulting in a mixture of crystalline ZrTiO 4 and XRD-amorphous phase can be compared with experimental conditions of Stubičar et al [13] and Kong et al [14]. We observed the simultaneous formation of the ZrTiO 4 and the XRD-amorphous phase for a mill rotation speed of 500 rpm, while Kong et al used a speed of 200 rpm and did not detected an amorphous phase by XRD.…”

“…This may resulted in an uncompleted solid state reaction giving nonstoichiometirc zirconia titanate. At high speed as used in the work of Stubičar et al (3200 rpm) [13], only an amorphous phase was formed. We can conclude that the most important parameter influencing the mechanochemical treatment of the ZrO 2 and TiO 2 oxide mixture was the rotation speed of the mill.…”

“…A thermal method in combination with low-energy mechanical treatment can be used to produce ZrTiO 4 through solid-state reaction of TiO 2 and ZrO 2 , but it needs heating cycles at temperatures around 1400 or even 1600 °C with additional mechanical grinding between repeated heating [4,9,10]. Mechanochemical synthesis using high-energy milling has been recognized in the field of materials science as a powerful tool in preparing novel materials at room temperature [11], but it is only occasionally used for the preparation of ZrTiO 4 ceramics [12][13][14]. Manik et al [12] obtained a small amount of nanocrystalline ZrTiO 4 dispersed in rutile TiO 2 (r-TiO 2 ) powder by annealing of a high-energy ball milled powder mixture of anatase TiO 2 (a-TiO 2 ):10 mol% monoclinic (m-ZrO 2 ), but a strong magnet has to be used to remove impurities before annealing.…”

“…Manik et al [12] obtained a small amount of nanocrystalline ZrTiO 4 dispersed in rutile TiO 2 (r-TiO 2 ) powder by annealing of a high-energy ball milled powder mixture of anatase TiO 2 (a-TiO 2 ):10 mol% monoclinic (m-ZrO 2 ), but a strong magnet has to be used to remove impurities before annealing. Using vial and balls made of WC-Co and agate, Stubičar et al prepared a fully amorphous material by high-energy ball-milling from an equimolar TiO 2 -ZrO 2 powder mixture [13]. The authors stated that with subsequent heat treatment of the amorphous material they obtained crystalline ZrTiO 4 , but with a lot of impurity.…”

Synthesis and Characterization of Crystalline Zirconium Titanate Obtained by Sol-Gel

“…Zirconium titanate is normally synthesized by solid-state reaction of oxide mixtures between ZrO 2 and TiO 2 at elevated temperatures (1200-1600°C) and long heating times and also requires post treatment such as energy-intensive grinding/milling procedures for powder formation and this process usually leads to inhomogeneous, coarse, and multiphase powders of poor purity (Lynch, 1972;Swartz, 1982;McHale et al, 1983;McHale et al, 1986;Parker, 1990;Christoffersen et al, 1992b;Park et al, 1996;Stubicar et al, 2001;Troitzsch et al, 2004;Dondi et al, 2006). ZrTiO 4 ceramics have the orthorhombic structure of α-PbO 2 (Blasse, 1966;Newnham, 1967) and belongs to the space group Pbcn.…”