In the present paper, we report successful synthesis of FeMoO4 hierarchical hollow spheres with 1.0 µm in diameter via a simple, rapid and reliable microwave-assisted solution-phase approach. The phases and morphologies of the products have been characterized by powder X-ray diffraction (XRD), energy dispersive spectrometry (EDS), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Some factors influencing the morphology of the final product have been investigated. These experiments indicate that the self-assembly of FeMoO4 nanoparticles at the water/gas interface is responsible for the formation of a hierarchical hollow structure.
