Developing a facile and general synthetic strategy toward particles with size, shape, and compositional control is of importance to nanotechnology applications. Ultrasonic spray synthesis (USS) is a continuous route to micro-and nanoscale particles with structural control, which are often difficult to obtain for inorganic solids with complex compositions or of metastable phases. This protocol describes the design and assembling of components for a simple reactor for USS. Components include a nebulizer, a nebulization chamber, a furnace, a furnace tube and the corresponding adapters, and a product collection apparatus. Details of our house-made components are provided as well as insights on material selection based on different synthetic requirements. We exemplify USS with a step-by-step procedure to single-crystalline NaSbO 3 nanoplates, and this procedure can be easily modified to accommodate other chemistries. The integration of USS and molten salt synthesis for single-crystalline NaSbO 3 nanoplates demonstrates the versatility of USS as a route to materials of different compositions, with shape and size control. With the incorporation of new chemical methods into USS, e.g., molten salt chemistry, topotactic transformations, and combustion chemistry, USS will remain a versatile, continuous flow platform for material syntheses.
Photoactive (IOI) inorganic/organic interface assemblies were prepared using an occlusion electrodeposition method. Poly-2,2′:5′,2′′-Terthiophene (PTTh) were the organic thin films that occluded each of CdS, TiO 2 , and Zn-doped WO 3 nanoparticles. The energy band gap structures were investigated using spectroscopic and electrochemical techniques. The obtained assemblies were investigated in aqueous solutions under both dark and illuminated conditions. The results were compared with the behavior of PTTh thin film. Oxygen played an important role in minimizing electron/hole recombination as was evident by observed very low photocurrent when oxygen was removed by nitrogen purge. Results show that PTTh/CdS gave the greatest photocurrent, followed by PTTh/Zn-WO 3 and PTTh/TiO 2 .
Inorganic/organic interfaces (IOI) consist of TiO2/PEDOT (poly 3,4-ethylenedioxythiophene) and [PMo12O40 ] 3− or MoO3/PEDOT were subject to photoelectrochemical studies in both aqueous nanosuspensions and in thin solid films. The effects PEDOT modifier caused on the photoelectrochemical behavior of the IOI were investigated using [Fe(CN)6] 4− as the photoactive hydrated electron donor agent. Results show that native PEDOT or PEDOT doped with MoO3 thin films increased charge storage capability evident by the high capacitive current. In the case of nano suspensions composed of TiO2/PEDOT the adsorption process of [Fe(CN)6] 3− (photolysis product) control of the photoactivity outcome of the IOI assemblies. TiO2/PEDOT shows a lower heterogeneous photochemical response than native TiO2 in short term photolysis times. At longer photolysis times the IOI shows photoactivity greater than that of native TiO2. The interface activities were explained by analyzing the IOI junction characteristics, such as electron affinity, work function and hole/electrons barrier heights. The aqueous nano-systems retained moderate stability as indicated by the reproducibility of their photocatalytic activities. Both [Fe(CN)6] 4− and PEDT contributed to the stability of native TiO2 surfaces.
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