The thermal reconstruction properties of ZnFe LDH that prepared by a facile hydrothermal method has been investigated. The ZnFe LDH was synthesized by urea hydrolysis in hydrothermal condition with zinc nitrate and iron nitrate as the precursor. In order to investigate its thermal reconstruction properties, the obtained products were calcined at 600 °C followed by rehydration treatment under the presence of NO3- ion solution. The properties of the natural, calcined, and reconstructed form of ZnFe LDH were investigated by X-ray diffraction, FT-IR, and TG-DTA analysis. The obtained result indicated that the calcined form of ZnFe LDH mainly composed of ZnO metal oxides. The calcined ZnFe LDH was successfully reconstructed.