Abstract: Fe(Ⅱ)-Al layered double hydroxides (Fe-Al LDHs) were prepared by the ultrasound-assisted co-precipitation method and used for the adsorption of uranium (Ⅵ) from aqueous solution. The effects of initial pH, adsorbent dosage, temperature, adsorption time and initial U(Ⅵ) ions concentration on adsorption of U(Ⅵ) were investigated. The prepared composites were characterized by SEM, FTIR, XRD and X-ray photoelectron spectroscopy (XPS). The experiment results indicate that the maximum adsorption occur at pH of 6 and the adsorption reach equilibrium within 120 min. Meanwhile the removal rate is up to 99.98% for initial U(Ⅵ) concentration of 10 mg/L and adsorbent dosage of 1.0 g/L at 25℃, and the maximum adsorption capacity for U(Ⅵ) ions is 117.13 mg/g. The experimental data fit well with the Langmuir isotherm model and pseudo-second-order kinetic model(R²≈1), Adsorption of U(Ⅵ) on Fe(Ⅱ)-Al LDH is primarily due to spontaneous endothermic reaction. The results of SEM、FTIR and XPS show that the structure of Fe(Ⅱ)-Al LDH has no change, chemisorption plays a major role and redox take subsidiary function.