Evaluation of Synthetic Methods for Bismuth(III) Oxide Polymorphs: Formation of Binary versus Ternary Oxides
Abstract
Hydrolysis of the bismuth oxido cluster [Bi38O45(O2CC3H5)24(DMSO)9] (A), dissolved in EtOH, with a diluted NaOH solution at ambient temperature using Teflon-lined vessels followed by heating of the amorphous product on a silver sheet gave pure γ-Bi2O3. The formation of Bi12SiO20 in addition to γ-Bi2O3 is observed when the hydrolysis of A is carried out in a glass vessel, which provides a low concentration of silicates as a result of glass corrosion. Hydrolysis of the cluster A under microwave-assisted heating in a Teflon-lined vessel gave β-Bi2O3, whereas Bi(NO3)3·5H2O (B) provided α-Bi2O3 and Bi12O17Cl2 was observed from BiCl3 (C). In glass vessels, alkaline induced hydrolysis of the precursors provided exclusively Bi12SiO20 as final product instead of the isomorphous metastable γ-Bi2O3. This observation is in contrast to recent literature reports. Powder X-ray diffraction studies, attenuated total reflection infrared spectroscopy, scanning electron microscopy, and energy dispersive X-ray spectroscopy were used to provide insight into the hydrolysis processes and into the concurring formation of the sillenite-type compound Bi12SiO20 instead of pure bismuth(III) oxide polymorphs.
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