Flower-like tetragonal iron selenide (β-FeSe) microstructures assembled from nanoplates have been successfully prepared using Se powder and FeCl3·6H2O as elemental precursors in the basic 1,2-propylene glycol (1,2-PG) solvent system by microwave irradiation for 1 h. The product was characterized by means of X-ray diffraction spectroscopy (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and energy-dispersive X-ray spectroscopy (EDX). The reaction mechanism and assembly process of the flower-like β-FeSe microstructures have been investigated and discussed, and a novel Se disproportionation-based reaction mechanism was proposed for the microwave-assisted synthesis of flower-like β-FeSe microstructures. In addition, ethylene glycol (EG) was also used as the reaction medium to investigate the influence of the different polyols on the size and structure of the product.
