Nanostructural evolution of II–VI semiconductors emerges as a hot research field because it offers a novel route for the synthesis of functional semiconductor nanomaterials. Here, we report a “top-down” process of structural evolution from two dimensional Cd2Se2(pa) hybrid structures to zero- or one- dimensional CdSe nanostructures. We firstly synthesized the Cd2Se2(pa) hybrid by a facile solvothermal reaction and determined the hybrid crystal structure through the Rietveld refinement based on the PXRD data. The (Cd2Se2)(pa) hybrid consists of [Cd2Se2] slabs sandwiched by coordinated n-propylamine layers. Then, we used this hybrid as a precursor to explore the “top-down” fabrication process of structural evolution from two dimensional layered structures to zero- or one- dimensional nanocrystals. It has been shown that various CdSe nanostructures including lamellar structures, nanoparticles, nanowires, and nanorods can be obtained through the pyrolysis of (Cd2Se2)(pa) hybrid precursor under different conditions. It is worth mentioning that the oriented attachment of nanoparticles has been observed during the pyrolysis process. Additionally, the variation of optical properties with structural evolution has been investigated in detail.
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