Abstract
A crystalline zirconium oxide sulfate compound with layer structure was synthesized by hydrothermal treatment of a mixture of zirconium hydroxide and sulfuric acid solution. The formation condition, crystallinity, composition and thermal changes of the compound crystals were investigated. It was found that the zirconium oxide sulfate layer compound is formed at temperatures above 150°C and pH values below 2. The crystallinity of the compound increased with the increase of both H2SO4 concentration and heat-treatment temperature. The crystals had a thin platelike shape 200-700nm in diameter and less than 20nm in width, and those synthesized at 220°C were sexangular. An electron diffraction pattern showed that there was a 6-fold symmetry axis in the direction perpendicular to the crystal with the lattice constant a equal to 0.632nm obtained by assuming a face of the crystals, and on the assumption of being hexagonal lattice. The ratio Zr: SO42- in the compound with high crystallinity was about three. The compound lost its interlayer water below 600°C, with the layer spacing decreased to a constant value of 1.048nm. Then, the compound was desulfurized at about 650°C, resulting in metastable tetragonal or monoclinic ZrO2 platelike skeletal grains.
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