Effects of Hydrothermal Processing on the Crystallinity and Morphology of the Precursor of In2O3

"The precursor of In2O3 was prepared by hydrolysis precipitation/hydrothermal method using In(NO3)3 solution as the feed material and ammonium hydroxide as the neutralizing agent. The crystallinity, morphology and particle size of the products were characterized by SEM, XRD, BET and LPSA. The results showed that the hydrolysis product consists of an aggregate of cubic In(OH)3 particles with a short rod morphology. In the hydrothermal process, the structure, morphology and size of the particles changes through the mechanisms of Ostwald ripening and phase transition, respectively. When the hydrothermal temperature was less than 280 ?, the Ostwald ripening process took place, which changed the morphology of the particles from short rods to cuboids through dissolution-recrystallization. When the hydrothermal temperature was higher than 280 ?, the processes of Ostwald ripening and phase transition took place successively. Firstly, the morphology of the particles changed from short rods to cuboids through Ostwald ripening, and then, the phase transition from cubic In(OH)3 to orthorhombic InOOH occurred and the morphology of the particles changed from cuboids to polyhedron. INTRODUCTIONDue to its excellent electrical conductivity and optical transparency, indium tin oxide (ITO) film has been wildly used in flat-panel display, solar cell, antistatic coating and EMI shielding (Medvedovski et al., 2008). Indium oxide powder is one of the fundamental materials for preparing ITO film. Along with the development of ITO targets of both high density and large size, high quality indium oxide powders, such as single phase, nano-size, spherical morphology and mono-disperse, have been in high demand (Nakashima and Kumahara, 2002; Betz et al., 2006; Kim et al., 2007). The main preparation methods for indium tin oxide or indium oxide powders include chemical precipitation (Nam et al., 2001; Xu and Yu, 2007), melt atomizing-combustion (Chen et al., 2000) and spray pyrolysis (Ogi et al., 2009). Among them, chemical precipitation has been preferred, since it is simple, easy to control and suitable for industrial scale-up. In chemical precipitation method, indium oxide powders were prepared through the following steps: firstly, indium hydrate precursor was precipitated from an indium salt solution by neutralization using an alkali, such as ammonia; and then, indium oxide (In2O3) powders can be obtained from the precursor through calcination (Li et al., 2006), or solvothermal method (Lee and Choi, 2005), or hydrothermal processing/roasting (Xu et al., 2005; Chen and Li, 2007), respectively. However, the indium oxide powders obtained by direct roasting are polycrystalline, dispersable with a wide size distribution (Liao, 2006). The disadvantages of the solvothermal method are high cost, complicated after-treatment processes, as well as bad performances of the powders (Udawatte and Yanagisawa, 2000). Therefore, among three methods of obtaining indium oxide from the hydrolysis precursor, the hydrothermal process/roasting method is the most feasible to synthesize high quality In2O3 powder with uniform crystallinity and size (Kim et al., 2002; Zhu et al., 2004; Xu et al., 2005; Xu et al., 2005; Chen and Li, 2007; Seetha et al., 2009). However, current research on hydrothermal process-roasting method has been limited to the synthesis of a certain ITO or In2O3 powders under specific conditions. A systematic study on the phase transition, as well as the change of the morphology and size of the particles in the hydrothermal process is still missing. In this paper, the effects of hydrothermal processing on the mineralogy, morphology and size of products were investigated. The results showed that the evolution of crystal structure, morphology and size in the hydrothermal process was affected through the mechanisms of Ostwald ripening and phase transition successively. These results are novel and have guidance for improving the hydrothermal process for In2O3"