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.
Photocatalysts offer an excellent opportunity to shift the global energy landscape from a fossil fuel-dependent paradigm to sustainable and carbon-neutral solar fuels. Oxynitride materials such as LaTiON are potential photocatalysts for the water splitting reaction due to their high oxidative stability and their narrow band gaps, which are suitable for visible light absorption. However, facile synthetic routes to metal oxynitrides with controlled morphologies are rare. Ultrasonic spray synthesis (USS) offers a facile method toward complex metal oxides which can potentially be converted to oxynitrides with preservation of the microsphere structures that typify the products from such aerosol routes. Here, La-Ti-O microspheres were facilely produced by USS and converted by ammonolysis to LaTiON microspheres with porous shells and hollow interiors. This particle architecture is accounted for by coupling suitable combustion chemistry with the aerosol technique, producing precursor particles where the La and Ti are well-mixed at small length scales; this feature enables preservation of the microsphere morphology during nitridation despite the crystallographic changes that occur. The LaTiON microspheres are comparable oxygen evolving photocatalysts to samples produced by conventional solid state methods. These results demonstrate the utility of USS as a facile, potentially scalable route to complex photocatalytic materials and their precursors with distinct morphologies.
Reaction pathways have been determined for the formation of two thermoelectric materials, bismuth telluride and lead telluride, fabricated by solution-phase, solid-state synthesis. The fabrication of these compounds by way of a modified polyol process has been investigated because this bottom-up approach has a proclivity for tailoring nanoscale features and has the potential to reduce manufacturing costs. These thermoelectric nanomaterials were characterized by powder X-ray diffractometry, scanning electron microscopy and energy-dispersive X-ray spectroscopy. By generating a range of samples as a function of temperature, mechanisms of formation were determined by mapping out changes in crystal structure, morphology and elemental composition. Growth mechanisms for both materials were compared to investigate which growth stages are unique to the compound being fabricated and which are common to the synthetic method. Findings showed that the formation of intermediate stages was dependent on variables beyond temperature and time, such as reduction rate, conjugate anion of the starting reagent and the reaction atmosphere. These types of experimental investigations of wet-chemical methods to fabricate nanomaterials with energy-related applications are fundamental to determine the feasibility of this approach to fabricate thermoelectric materials with reduced production costs and improved energy transport properties.
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