Ca-Al and Ca-Fe layered double hydroxides (LDHs) were successfully synthesized from chicken eggshells by an ultrasonic wave assistant method. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FT-IR) techniques. XRD and TEM analyses showed that the 4Ca-Al LDHs were of high purity but other samples were not. The present study provides a simple, efficient and environmental friendly method to obtain LDHs from biowaste eggshells, in which additional alkaline solution is not required for synthesis. Moreover, eggshells provide all the requisite bivalent metal ions, which are needed to form layered double hydroxides. (C) 2011 Elsevier B.V. All rights reserved.