Phase Transformation and Microstructure of Zn₂Ti₃O₈ Nanocrystallite Powders Prepared Using the Hydrothermal Process

Abstract

This paper examines the phase transformation and microstructure of Zn₂Ti₃O₈ nanocrystallite powders prepared using the hydrothermal process that includes TiCl₄ and Zn(NO₃)₂·6H₂O as the initial materials. Differential thermal analysis, X-ray diffraction, transmission electron microscopy (TEM), selected area electron diffraction, nanobeam electron diffraction, and high resolution TEM were utilized to characterize the transition behavior of zinc titanate precursor powders after calcination. Nanocrystalline Zn₂Ti₃O₈ powders with a size range of about 5.0 to 8.0 nm were obtained when the precursor powders were calcined at 773 K (500 °C) for 1 hour. When the zinc titanate precursor powders were calcined at 1073 K (800 °C) for 1 hour, the cubic crystal of Zn₂Ti₃O₈ with a _o = 0.8399 ± 0.0003 nm still remained the predominant crystalline phase and the crystallite size increased to 20.0 nm. In addition, ZnTiO₃ phase first appeared because of the 13.8 pct of Zn₂Ti₃O₈ decomposition when the zinc titanate precursor powders were calcined at 1073 K (800 °C) for 1 hour. When the zinc titanate precursor powders were calcined at 1073 K (800 °C) for 9 hours, the Zn₂Ti₃O₈ crystallites grew continuously to 80.0 nm and enhanced the crystallinity. When the precursor powders were calcined at 1273 K (1000 °C) for 1 hour, Zn₂TiO₄ crystallites with a _o = 0.8461 ± 0.0002 nm were the predominant crystalline phase.