Development of mesoporosity in scandia-stabilized zirconia: particle size, solvent, and calcination effects

We present the mechanisms of formation of mesoporous scandia-stabilized zirconia using a surfactant-assisted process and the effects of solvent and thermal treatments on the resulting particle size of the powders. We determined that cleaning the powders with water resulted in better formation of a mesoporous structure because higher amounts of surfactant were preserved on the powders after washing. Nonetheless, this resulted in agglomerate sizes that were larger. The water-washed powders had particle sizes of >5 μm in the as-synthesized state. Calcination at 450 and 600 °C reduced the particle size to ∼1-2 and 0.5 μm, respectively. Cleaning with ethanol resulted in a mesoporous morphology that was less well-defined compared to the water-washed powders, but the agglomerate size was smaller and had an average size of ∼250 nm that did not vary with calcination temperature. Our analysis showed that surfactant-assisted formation of mesoporous structures can be a compromise between achieving a stable mesoporous architecture and material purity. We contend that removal of the surfactant in many mesoporous materials presented in the literature is not completely achieved, and the presence of these organics has to be considered during subsequent processing of the powders and/or for their use in industrial applications. The issue of material purity in mesoporous materials is one that has not been fully explored. In addition, knowledge of the particle (agglomerate) size is essential for powder handling during a variety of manufacturing techniques. Thus, the use of dynamic light scattering or any other technique that can elucidate particle size is essential if a full characterization of the powders is needed for achieving postprocessing effectiveness.