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Zn-doped MgAl layered double hydroxides (LDHs) with M2+/M3+=2 and different molar ratios of Mg/Zn have been synthesized by modified homogeneous co-precipitation method and characterized by powder x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), fourier transform infrared spectrum (FT-IR) and thermogravimetry and differential thermal analysis (TG-DTA) techniques.The as-synthesized plate-like LDHs nanoparticles have an average diameter around 90nm and thickness about 20nm.