Study on the microstructure and properties of nanosized stannic oxide powders

Abstract

Stannic oxide xerogel was prepared by a forced hydrolysis method using SnCl 4 as the precursor. The average grain sizes of the nanosized stannic oxide powders varied with the sintering temperatures. The powders were characterized by several different physico-chemical techniques. TEM was employed for the direct observation on grain sizes, shape and state of aggregation of the particles. XRD technique was used for the determination of the crystalline structure. Microstructural parameters of average crystallite size (<D>) and mean-square root microstrain (<ε 2> 1/2) for the samples were calculated from the broadened values of the half-peak intensity of XRD. The atomic ratio between oxygen and tin in the surface region of the particles was estimated through the analysis of XPS. Attributing to lots of oxygen vacancies in the surface region of the nanoparticulates and the ‘trapped electrons’ in the vacancies, an ESR signal was observed in the sample sintered at 300 °C for 2 h. FTIR of the powders showed that intensity of the transverse optical mode of Sn-O stretching vibration increased with the sintering temperature while the bending vibration of O-Sn-O showed a blue shift. For Raman spectra, very important spectral characteristics such as variations of intensity and width of the bands were observed. A new Raman vibrational band located at 572 cm −1 was identified in the samples of nanosized stannic oxide powders. Variation of these spectroscopic properties were strongly affected by grain size, shape and state of aggregation of the nanosized particulates.