Novel hierarchical ZnO nanostructures, porous ZnO nanobelts, and nanoparticle chains are prepared from a precursor of synthetic bilayered basic zinc acetate (BLBZA) nanobelts. BLBZA nanobelts are obtained by a simple synthetic route under mild conditions. X‐ray diffraction, scanning electron microscopy, transmission electron microscopy, infrared spectroscopy, and thermal analysis are used to characterize the BLBZA nanobelts and ZnO nanostructures. The obtained BLBZA precursor consists of a lamellar structure with two interlayer distances of 1.33 and 2.03 nm, exhibits a beltlike morphology, and has widths of 200 to 600 nm, thicknesses of 10 to 50 nm, and lengths of up to 50 μm. Refluxing an aqueous dispersion of BLBZA nanobelts at 120 °C for 12 h leads to the formation of well‐defined hierarchical ZnO nanostructures. The time‐dependent shape‐evolution process suggests that spindlelike ZnO particles form first, and then the ringlike nanosheets grow heterogeneously on the backbone of these spindles. In addition, calcination in air can remove ligand molecules and intercalated water molecules from BLBZA nanobelts, resulting in the formation of porous ZnO nanobelts and nanoparticle chains. The BLBZA nanobelts serve as templates during the transformation to form ZnO beltlike nanoparticle chains without morphological deformation. Photoluminescence results show that both the as‐synthesized hierarchical ZnO nanostructures and porous ZnO nanobelts show a narrow and sharp UV emission at 390 nm and a broad blue–green emission at above 466 nm when excited by UV light.

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Complex Sb 2 S 3 and Sb 2 Se 3 nanostructures with a sheaf-like hierarchical morphology were prepared on a large scale at 180 °C by a simple hydrothermal method in the presence of poly(vinyl pyrrolidone) (PVP). X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and high-resolution transmission electron microscopy were used to characterize the products. The results indicate that threedimensional Sb 2 S 3 and Sb 2 Se 3 complex nanostructures were constructed by fractal splitting growth. The timedependent shape-evolution process suggests that initial stages of the growth comprise nanorod seeds. These PVP-stabilized nanorods develop in subsequent growth stages to a dumbbell structure and complete their development as a closed sphere with an equatorial notch. It has been demonstrated that PVP plays a key role in the formation of such hierarchical nanostructures. Ultraviolet-visible-near-infrared spectroscopy was further employed to estimate the band gap energy of the obtained products. The measurements of the optical properties revealed that the obtained materials have a band gap of 1.56 eV for Sb 2 S 3 and 1.13 eV for Sb 2 Se 3 . Our work may shed some light on the design of other well-defined complex nanostructures, and the as-grown architectures may have potential applications.