derived from BaCO 3 . Small particle size has been shown to suppress a martensitic phase transition, and in this context microwave plasma synthesis appears rapid enough to prevent particle sintering and subsequent transition to the monoclinic phase. Prolonged exposure (1 h) to an O 2 or Ar plasma of either the orthorhombic or monoclinic phases did not result in a phase change as judged by powder XRD.In conclusion, we have used a simple microwave plasma reactor for reproducible bulk synthesis of several ternary niobate and titanate phases. MIP synthesis does not require direct interaction between a solid and microwave radiation and is, therefore, amenable to any solid-state reaction. Importantly, for some reactions the plasma can also be used to heat solids into a temperature regime where additional dielectric heating can occur, resulting in a local temperature much greater than the equilibrium MIP temperature.
ExperimentalPrecursor oxides (Nb 2 O 5 , TiO 2 , and BaO 99.99 %) and carbonates (Li 2 CO 3 99.99 %, Na 2 CO 3 99.995 %, K 2 CO 3 99.995 %, CaCO 3 99.995+ %, BaCO 3 99.999 %, and PbCO 3 99.99+ %) were purchased from Aldrich and used as received. Plasma gases (Ar and O 2 ) were purchased from BOC. In a typical synthesis, a total mass of 2 g of precursors was ground in a drybox and pressed at 10 tonnes into a 13 mm pellet, and the pellet was transferred to the microwave apparatus via a desiccator. The pellet was placed in an alumina boat and exposed to a plasma at 13 mbar (1mbar = 10 2 Pa), 900 W, and a gas flow rate of 200 cm 3 min -1 for argon and 142 cm 3 min -1 for dioxygen. After microwave plasma irradiation, products were transferred directly into a drybox for storage. Products were characterized by powder X-ray diffraction (Philips 1800 diffractometer PH 03, with Cu Ka radiation (k = 1.54 Å) in reflection mode), scanning electron microscopy (FEI Sirion 200), and analytical transmission electron microscopy (FEI CM200 FEGTEM) that included electron energy loss spectroscopy (EELS). the synthesis of tubular nanomaterials has aroused worldwide interest -both in fundamental studies, and for their potential application in, for example, chemical sensors, and as catalysts and storage and/or release systems. [2][3][4][5] Zinc oxide (ZnO), a II-VI compound semiconductor, has many remarkable properties. The wide direct bandgap of ZnO (3.37 eV) and large exciton binding energy (∼ 60 meV at room temperature)