Nano-architectural complexity of zinc oxide nanowall hollow microspheres and their structural properties

Zinc oxide (ZnO) hollow spheres with defined morphology and micro-/nanostructure are prepared by a hydrothermal synthesis approach. The materials possess fine-leaved structures at their particle surface (nanowall hollow micro spheres). Morphology control is achieved by citric acid used as an additive in variable relative quantities during the synthesis. The structure formation is studied by various time-dependent ex situ methods, such as scanning electron microscopy, x-ray diffraction, and Raman spectroscopy. The fine-leaved surface structure is characterized by high-resolution transmission electron microscopy techniques (HRTEM, STEM), using a high-angle annular dark field detector, as well as by differential phase contrast analysis. In-depth structural characterization of the nanowalls by drop-by-drop ex situ FE-SEM analysis provides insight into possible structure formation mechanisms. Further investigation addresses the thermal stability of the particle morphology and the enhancement of the surface-to-volume ratio by heat treatment (examined by N₂ physisorption).